LITHIUM-1-BUTANIDE
n-Butyllithium
CAS: 109-72-8
Molecular Formula: C4H9Li
LITHIUM-1-BUTANIDE - Names and Identifiers
| Name | n-Butyllithium |
| Synonyms | N-BULI butyl-lithiu LITHIUMBUTYL BUTYLLITHIUM N-BUTYLLITHIUM Lithiumn-butyl n-Butyllithium LITHIUM-1-BUTANIDE Butyllithium solution ButyllithiuminhexaneM |
| CAS | 109-72-8 |
| EINECS | 203-698-7 |
| InChI | InChI=1/C4H9.Li/c1-3-4-2;/h1,3-4H2,2H3;/rC4H9Li/c1-2-3-4-5/h2-4H2,1H3 |
LITHIUM-1-BUTANIDE - Physico-chemical Properties
| Molecular Formula | C4H9Li |
| Molar Mass | 64.06 |
| Density | 0.68g/mLat 20°C |
| Melting Point | -95 °C |
| Boling Point | 80°C |
| Flash Point | 10°F |
| Water Solubility | vigorous reaction |
| Solubility | Miscible with diethyl ether and cyclohexane. |
| Appearance | liquid |
| Specific Gravity | 0.695 |
| Color | yellow |
| Odor | Odor of the solvent |
| Exposure Limit | ACGIH: TWA 50 ppm (Skin)OSHA: TWA 500 ppm(1800 mg/m3)NIOSH: IDLH 1100 ppm; TWA 50 ppm(180 mg/m3) |
| BRN | 1209227 |
| Storage Condition | 2-8°C |
| Sensitive | Air & Moisture Sensitive |
| Physical and Chemical Properties | Density 0.68 boiling point 60-80°C flash point -21°C water-soluble vigolous reaction |
LITHIUM-1-BUTANIDE - Risk and Safety
| Risk Codes | R17 - Spontaneously flammable in air R34 - Causes burns R51/53 - Toxic to aquatic organisms, may cause long-term adverse effects in the aquatic environment. R62 - Possible risk of impaired fertility R65 - Harmful: May cause lung damage if swallowed R67 - Vapors may cause drowsiness and dizziness R63 - Possible risk of harm to the unborn child R35 - Causes severe burns R11 - Highly Flammable R15 - Contact with water liberates extremely flammable gases R50/53 - Very toxic to aquatic organisms, may cause long-term adverse effects in the aquatic environment. R66 - Repeated exposure may cause skin dryness or cracking |
| Safety Description | S6 - Keep under ... (there follows the name of an inert gas). S9 - Keep container in a well-ventilated place. S16 - Keep away from sources of ignition. S26 - In case of contact with eyes, rinse immediately with plenty of water and seek medical advice. S36/37/39 - Wear suitable protective clothing, gloves and eye/face protection. S45 - In case of accident or if you feel unwell, seek medical advice immediately (show the label whenever possible.) S61 - Avoid release to the environment. Refer to special instructions / safety data sheets. S62 - If swallowed, do not induce vomitting; seek medical advice immediately and show this container or label. S46 - If swallowed, seek medical advice immediately and show this container or label. S43 - In case of fire use ... (there follows the type of fire-fighting equipment to be used.) S60 - This material and its container must be disposed of as hazardous waste. S33 - Take precautionary measures against static discharges. S29 - Do not empty into drains. S5 - Keep contents under ... (there follows the name of a liquid). |
| UN IDs | UN 3399 4.3/PG 1 |
| WGK Germany | 3 |
| FLUKA BRAND F CODES | 3-10 |
| TSCA | Yes |
| HS Code | 29319090 |
| Hazard Class | 4.3 |
| Packing Group | I |
| Toxicity | There is little toxicity data available for the butyllithiums; for data on ether and hydrocarbon solvents, see the appropriate LCSSs. |
LITHIUM-1-BUTANIDE - Quenching method
Open Data Unverified Data
slowly pour into tetrahydrofuran with a small amount of dry ice, slowly add twice the amount of molar ethanol, then add water to dilute, finally add dilute HCl until the solution becomes clear, and pour into the corresponding waste liquid barrel in the floor fume hood.
Quenching treatment needs to consider:
1) Choose a suitable quenching reagent, and fully consider the stability of the product and the difficulty of post-treatment;
2) If the quenching process will release a lot of heat, it must be quenched under cooling;
3) Don't rely too much on the literature without monitoring the response. The reaction can only be quenched when TLC or other analytical means show the end of the reaction;
4) If possible, post-treatment should be carried out as soon as possible after quenching.
Last Update：2024-04-12 10:21:36
LITHIUM-1-BUTANIDE - Overview
n-butyl lithium is a colorless or yellowish transparent liquid, stable at room temperature, and heat to eliminate lithium hydride. It decomposes in water, dissolves in hydrocarbons and ethers, forms complexes with ethers, amines and thioethers, uses n-hexane as solvent, and has a density of 0.675g /ml. Generally, dilute solutions with molar concentrations ranging from 1.0M-1.3M are prepared with mass percentage concentrations ranging from 9% to 13%. They are widely used in organic catalytic reactions of pharmaceutical intermediates, liquid crystal monomers, pesticides and rubber industries.
Using n-butyl lithium (BuLi) as the initiator, tetrahydrofuran (THF) as the structure regulator, tin tetrachloride (SnCl4) as the coupling agent to synthesize integrated rubber SIBR, integrated rubber SIBR is a new type of rubber used for treads. Its notable feature is that the molecular chain is composed of segments with multiple structures. The segments with different structures provide different properties to the rubber, at the same time, it can also reduce the rolling friction resistance and improve the wear resistance of the tire; while the rigid chain segment increases the wet grip of the rubber and improves the safety of the tire on wet and slippery roads, which makes SIBR the most comprehensive performance so far. Diolefin rubber. Due to its excellent comprehensive performance, SIBR is considered as the hot rubber of this century and has a bright development prospect.
Preparation method of ether solution
Under the protection of anhydrous and oxygen-free nitrogen, in a 500 ml dry three-neck flask equipped with a stirrer, a low-temperature thermometer, an air duct, a drying tube and a drip funnel, add 200 ml of anhydrous ether and cut 8.6g (1.25 mol) of lithium wire, and drop 30 drops of 68.5g (0.50 mol) of n-bromobutane and 100 ml of anhydrous ether under stirring. When it is cooled to -10 ℃ in the dry ice-acetone bath, the reaction starts when the solution becomes turbid and the lithium wire shows bright spots with metallic luster. The remaining n-bromobutane solution was added within 30 minutes. Then slowly warm to 0-10 ℃, and continue stirring for 1-2 hours. Filter through a glass tube stuffed with glass filaments under nitrogen protection, and transfer the ether solution of n-butyl lithium to a pre-rinsed nitrogen container for storage, with a yield of 80-90%.
The preparation method of n-hexane solution
Under nitrogen protection, add 120 ml of n-hexane solution, 4.8 grams (0.7 moles) of lithium wire, and drop 29.6 grams (0.32mmol) of n-butane to a three-mouth flask equipped with a dropping funnel, a thermometer and a condenser tube., Slowly raise the temperature and maintain a steady boiling. It takes about 1 hour to complete the dropwise addition, continue the reflux reaction for 1.5 hours, cool, stand overnight, filter under.
precautions
N-butyl lithium is sensitive to air and water. Please store the product in a closed, dry, low temperature (2-8 ℃) environment.
Long-term storage may produce a small amount of turbidity, which is a normal phenomenon and does not affect the use of the product.
When using a syringe to extract the solution, a nitrogen balloon should be connected with an injection needle at the mouth of the bottle to balance the pressure change when n-butyl lithium is sucked out.
The reaction system of n-butyl lithium needs to maintain a nitrogen environment to prevent air and water from entering. The solvent used should be anhydrous or ultra-dry solvent.
Last Update：2023-08-17 17:13:27
LITHIUM-1-BUTANIDE - Safety Information
Open Data Unverified Data
Store in a cool, dry, well-ventilated warehouse, away from fire and heat sources. The temperature of the warehouse shall not exceed 30 ℃ and the relative humidity shall not exceed 80%. The package must be sealed and must not be exposed to moisture. Should be stored separately with acids, alcohols, etc., do not mix storage. It should not be stored in large quantities or for a long time. Explosion-proof lighting and ventilation facilities shall be adopted. It is forbidden to use mechanical equipment and tools that are easy to produce sparks. The storage area should be equipped with leakage emergency treatment equipment and suitable containment materials.
Emergency response to leakage
Quickly evacuate the personnel from the leakage pollution area to the safety area, isolate them and strictly restrict access. Cut off the fire source. It is recommended that emergency personnel wear self-contained positive pressure breathing apparatus and protective clothing. Do not touch the leak directly. Cut off the leak source as much as possible.
Small leakage: Absorb with sand, vermiculite or other inert material.
A large number of leaks: build a dam or dig a pit for containment. Transfer to tanker or special collector with explosion-proof pump, recycle or transport to waste treatment site for disposal.
Protective measures
Respiratory protection: It is recommended to wear a self-inhaling filtering respirator (full face mask) when exposed to poisons. In case of emergency rescue or evacuation, it is recommended to wear air respirator.
Eye protection: protection has been made in respiratory system protection.
Body protection: Wear tape protective clothing.
Hand protection: Wear rubber gloves.
Other: Smoking is strictly prohibited on the job site. After work, shower and change clothes.
First aid measures
Skin Contact: Immediately remove contaminated clothing and rinse with plenty of flowing water for at least 15 minutes. Seek medical attention.
Eye Contact: Immediately lift the eyelid and rinse thoroughly with plenty of flowing water or saline for at least 15 minutes. Seek medical attention.
Inhalation: Quickly leave the site to fresh air. Keep the airway unobstructed. If breathing is difficult, give oxygen. If breathing stops, give artificial respiration immediately. Seek medical attention.
ingestion: gargle with water and drink milk or egg white. Seek medical attention.
Last Update：2024-04-09 19:43:38
LITHIUM-1-BUTANIDE - Security information
Open Data Unverified Data
1. Flammability: n-butyl lithium is a strong combustible substance that can burn in the air and produce flammable vapors. It should be kept away from open flames, high temperatures, and sources of ignition.
2. Corrosiveness: n-butyl lithium has strong corrosiveness and can react violently with water, releasing intense and rapid hydrogen gas. When handling, avoid contact with environments with high moisture or humidity.
3. Irritation to skin and eyes: n-butyl lithium is irritating to the skin and eyes. If you accidentally come into contact with n-butyl lithium, you should immediately rinse with plenty of water and seek medical help.
4. Toxicity: n-butyl lithium has low toxicity to the human body. However, correct operating procedures should still be followed during use and handling to avoid inhaling its vapors or coming into contact with the skin.
5. Packaging and storage: n-butyl lithium is usually stored in an anhydrous solution or organic solvent form and should be stored in a closed, dry, and cool place. When storing, it should be separated from other flammable substances, oxidants, and acidic substances, and avoid direct sunlight exposure.
In summary, for the use and handling of n-butyl lithium, it is necessary to follow correct operating procedures and pay attention to personal protective measures, such as wearing protective glasses, gloves, and goggles, to ensure safety and minimize risks.
Last Update：2024-04-09 19:43:38
LITHIUM-1-BUTANIDE - Nature
| melting point | -95 °C |
| boiling point | 80 °C |
| density | 0.68 g/mL at 20 °C |
| flash point | 10 °F |
| storage conditions | 2-8°C |
| solubility | Miscible with diethyl ether and cyclohexane. |
| morphology | liquid |
| color | yellow |
| Specific gravity | 0.695 |
| Odor | Odor of the solvent |
| water solubility | vigorous reaction |
| sensitivity | Air & Moisture Sensitive |
| hydrolysis sensitivity | 8: reacts rapidly with moisture, water, protic solvents |
| BRN | 1209227 |
| EPA chemical information | Lithium, butyl- (109-72-8) |
Last Update：2024-04-10 22:29:15
LITHIUM-1-BUTANIDE - Take
the syringe is filled with nitrogen, injected into the n-butyl lithium bottle, then the n-butyl lithium is sucked, and injected into the reaction system filled with nitrogen in advance (of course, this system includes a constant pressure dropping funnel), and then the plug is added with n-butyl lithium dropwise.
After a small amount is directly inhaled with a syringe, it is slowly added with a syringe, of course, to ensure that the container is filled with nitrogen. Be careful to prepare a triangular bottle containing a small amount of dry tetrahydrofuran or petroleum ether and wash the used syringe.
Last Update：2024-04-10 22:29:15
LITHIUM-1-BUTANIDE - Reference Information
| LogP | 1.25-2.31 |
| NIST chemical information | information provided by: webbook.nist.gov (external link) |
| EPA chemical substance information | information provided by: ofmpeb.epa.gov (external link) |
| Overview | n-butyl lithium is a colorless or yellowish transparent liquid that is stable at room temperature and is heated to eliminate lithium hydride. Water decomposition, soluble in hydrocarbons and ethers, and ether, Amine and sulfide into a complex, with n-hexane as solvent, density 0.675g /ml. Generally formulated to a molar concentration of 1.0M-1.3M range of dilute solution, its mass percentage concentration between 9%-13%, widely used in pharmaceutical intermediates, liquid crystal monomer, pesticide and rubber industry organic catalytic reaction. with n-butyl lithium (BuLi) as initiator, tetrahydrofuran (THF) as structure modifier, tin tetrachloride (SnCl4) as coupling agent, integrated Rubber SIBR is a new type of rubber for tread. Its remarkable feature is that the molecular chain is composed of segments of various structures, and the segments of different structures provide different properties to the rubber, the chain segment with strong flexibility makes the rubber have excellent low-temperature performance, and can also reduce the rolling friction resistance and improve the wear resistance of the tire. The rigid chain segment increases the wet grip of the rubber, to improve the safety of the tire in the wet road, which makes SIBR the most comprehensive performance of the Diene Rubber. Due to its excellent comprehensive properties, SIBR is considered as a hot rubber in this century and has a bright future. Method of preparation of diethyl ether solution under the protection of anhydrous and oxygen-free nitrogen, in a 500 ml dry three-necked flask equipped with a stirrer, a cryo-thermometer, an air duct, a drying tube and a dropping funnel, add 200 of anhydrous ether and 8.6g (1.25 mol) of cut lithium wire, A solution of 68.5g (0.50 mol) of n-bromobutane and 100 of anhydrous diethyl ether was added dropwise with stirring. Cooling to -10 °c in a dry ice-acetone bath indicated the start of the reaction when the solution became cloudy and a bright spot of metallic luster appeared on the lithium wire. The remaining n-bromobutane solution was added over 30 minutes. It was then slowly warmed to 0-10 °c and stirred for another 1-2 hours. The solution of N-butyllithium in diethyl ether was transferred to a container previously flushed with nitrogen for storage by filtration through a glass tube filled with glass strands under nitrogen in 80-90% yield. Method for preparation of n-hexane solution under the protection of nitrogen, 120 of n-hexane solution, 4.8g (0.7 mol) of lithium wire were added to a three-necked flask equipped with a dropping funnel, a thermometer and a condenser, add 29.6G (0.32mmol) of n-butyl chloride Dropwise, slowly raise the temperature, maintain stable boiling, it takes about 1 hour to complete the dropwise addition, continue the Reflux reaction for 1.5 hours, cool, stand overnight, under the protection of nitrogen, the filtrate was filtered and stored by flushing. Note n-butyl lithium is sensitive to air and water, please store the product in a closed, dry, low temperature (2-8 ℃) environment. long-term storage may produce a small amount of turbidity, which is a normal phenomenon and does not affect the use of the product. when using a syringe to extract the solution, a nitrogen balloon should be connected with an injection needle at the mouth of the bottle to balance the pressure change when the n-butyl lithium is aspirated. The reaction system of n-butyl lithium needs to maintain a nitrogen environment, To block the ingress of air and water, the solvent used should be anhydrous or ultra-dry. |
| quenching method | slowly pour into tetrahydrofuran with a small amount of dry ice, slowly add an excess of 1-mole ethanol, then dilute with water, finally add dilute HCl until the solution becomes clear, and pour into the corresponding waste liquid bucket in the landing fume hood. Quenching treatment need to consider: 1) select the appropriate quenching reagent, to fully consider the stability of the product and the ease of post-treatment; 2) If the quenching process will be a large amount of heat, quenching must be performed with cooling; 3) do not rely too much on literature and do not monitor the reaction. The reaction can be quenched only when TLC or other analytical means show the end of the reaction; 4) if possible, work-up should be carried out as soon as possible after the quenching. |
| preparation of butyl lithium | under the protection of argon, add 3L of n-hexane (or petroleum ether at 60-90 °c) to a 3 ml flask, wash 140g(20mol) of lithium metal with n-hexane (or petroleum ether at 60-90 ℃), put on disposable gloves, tear the lithium metal into small pieces quickly, add them into a 5000ml three-mouth bottle, and load them with mechanical stirring, ice salt bath cooling to about 0 degrees (note that the temperature is not too low, otherwise the initiation is relatively slow), to which the drop of 0.25g(10mol) chlorobutane, the temperature control is below 15 degrees (note that after the reaction is initiated, it should be slowly added at the beginning, the reaction is more exothermic, pay special attention to not flush), after adding, ice salt bath temperature control below 15 degrees and continue to stir for 2 hours, Then the ice salt bath was removed, stirred at room temperature for 1 hour, then changed to reflux device, gradually heated and refluxed for 4-5 hours, cooled to room temperature, and left to settle overnight. The supernatant was butyllithium solution, the storage bottle was pressurized with argon, the residue was stirred with 2L of solvent, settled overnight, and the supernatant was combined into a butyllithium solution for use. Residue treatment: place the upper residue with a bottle in a pot filled with sand, place it in a safe place, and expose it to air for 1-2 months (without spontaneous combustion), when the solid in the system turns white, it comes out immediately, and it is enough to pour water on the open space far above. If the local climate is relatively humid, the first few days should be added to the bottle mouth on both sides of the drying tube. If the reaction bottle is used urgently, after the transfer of the n-butyl lithium solution, it can be cooled in an ice salt bath under the protection of argon, and treated slowly by adding tert-butyl alcohol dropwise. |
| butyl lithium titration and calibration method | butyl lithium must be calibrated before use, double titration method is more cumbersome, generally not, it can be titrated by a single titration method. The specific methods are as follows: 1) titration reagent: 1mol/L sec-butanol/xylene solution (sec-butanol and xylene must be dried with activated 5A Molecular sieve) 2) indicator: 2,2 '-bipyridine 3) solvent: xylene (to be dried with activated 5A Molecular sieve) 4) operation method: under the protection of argon, add a magnet, 20ml xylene, a small amount of indicator, to a 100ml triplex bottle with a flip plug, then use a syringe with a precision scale of 2ml to accurately measure 2ml of butyl lithium and quickly transfer it into the bottle (the air in the syringe needs to be replaced with argon, and the argon in the syringe needs to be excluded when the butyl lithium is extracted, and in the butyl lithium solution back and forth pumping several times, so as to avoid the micro amount of water and air in the syringe affect the accuracy of titration), the system becomes purple red, then wash the same syringe (the purpose of using the same syringe is to reduce the titration error), blow dry, and wash two to three times with titrant, accurate titration titration of titrant system mutation to yellow, this is the end point of titration. 5) If the titration is repeated once and the error is less than 2%, the result can be considered accurate. 6) titration results: Titration dose (ml)/2 is the molar concentration of butyl lithium note: 1) n-butyl lithium is extremely spontaneous combustion in air, when measuring, the tip of the needle in the air will fire Mars. 2) the whole process must be protected with argon, especially the need to pay attention to safety. 3) when butyl lithium fires, it is necessary to use sand to extinguishing the fire. At ordinary times, sand for fire fighting should be provided at a place within reach. 4) when preparing and using butyl lithium, it is best not to operate alone, so as to avoid accidents, a person can not handle. |
| access | The syringe was filled with nitrogen, injected into the n-butyl lithium bottle, and then absorbed n-butyl lithium, it is injected into a reaction system previously filled with nitrogen (This system includes, of course, a constant-pressure dropping funnel), and then n-butyl lithium is added dropwise by a stopcock. After a small amount is directly inhaled with a syringe, the syringe is slowly added dropwise, and of course, the container must be filled with nitrogen. Be careful to remember to prepare a triangle bottle containing a small amount of dry tetrahydrofuran or petroleum ether and wash the used syringe. |
| precautions for use | n-butyl lithium is a versatile anionic polymerization initiator, explosion and fire caused by butyl lithium have been reported frequently in recent years. So in the use of butyl lithium in the experiment how to operate as far as possible to avoid the occurrence of these tragedy? (1) butyl lithium is highly spontaneous when exposed to air, and the needle tip will emit Mars in air when measured; (2) inert gas shall be used for protection during the whole process, special attention should be paid to safety; (3) when butyl lithium fires, sand should be used to extinguishing the fire. At ordinary times, it is necessary to prepare sand for fire fighting in a place within reach; (4) when preparing and using butyl lithium, it is best not to be operated by one person alone, so as not to be able to be handled by one person in case of accident; (5) n-butyl lithium is a particularly strong nucleophilic reagent, which can be used as an initiator for anionic polymerization. Plastic or rubber containers should be avoided and kept protected from light and water at low temperature; (6) the reaction system and solvent using butyl lithium should be strictly anhydrous and oxygen-free; (7) do not dip or drip butyl lithium onto flammable substances (e. G., in the acetone cold bath of dewapin); (8) in the process of taking butyl lithium, the needle will be blocked (when the air humidity is large, the rubber dust of the solid or the reverse plug in the front of the needle is inserted into the needle hole), so it is necessary to be calm, tell the person accompanying you to handle the operation properly; (9) once butyl lithium drops on the table or the ground, do not use Nervousness, immediately cover with asbestos or sand. Do not drip into clothes or solvent; (10) when the dosage is large, it is recommended to use dry and clean stainless steel catheters directly, butyl lithium is slowly dropped into the reaction system through a small positive pressure of an appropriate inert gas that can control the flow rate, and the measure of interrupting at any time is to draw the stainless steel pipe from below the liquid level of butyl lithium to above the liquid level in a timely manner; (11) the addition rate of butyl lithium should be strictly controlled, if the weather is slightly higher, the part of the frozen bottle exposed above the surface of the dry ice-acetone bath will have a very thick frost on its outer wall, and it is basically impossible to clearly observe the speed and speed of the reaction in the reaction bottle. |
| purpose | polymerization catalyst, hydrocarbon agent. used as chemical intermediates and linking agent butyl lithium is widely used in organic synthesis, increasing carbon chain, and is a relatively basic laboratory product. 1, metallization reaction: R-H n-Butyl-Li → R-Li Butane, the generated substance alkyl lithium can react with a variety of substances. 2. Direct metallization reaction: an aromatic compound to which a substituent is attached is reacted with n-butyl lithium, and lithium metal may be attached to the aromatic compound. 3, nucleophilic addition and substitution reaction 4, halogen-metal substitution n-butyl lithium solution is mainly used as anionic polymerization initiator in the synthesis of organic reaction of pharmaceutical intermediates, at the same time, it is also used in synthetic rubber, fragrance synthesis, liquid crystal materials and other industries and fields. n-butyl lithium (n-C4H9Li) is mainly used as an organic reaction catalyst and is widely used in the organic catalytic reactions of drug intermediates, liquid crystal monomers, pesticides and rubber industry. |
| production method | under nitrogen, the pure ether and the cut lithium wire were cooled to -10 °c, and the stirring was started, A solution of bromobutane in diethyl ether was added dropwise. After completion of the dropwise addition, the reaction was slowly warmed to 0-10 ° C., reacted for 1-2H, and filtered to obtain n-butyl lithium ether solution (commercial product), with a yield of 80%-90%. |
| category | spontaneous combustion in water |
| explosive hazard characteristics | Possible explosion with styrene polymerization |
| flammability hazard characteristics | concentration greater than 20% in the air spontaneous combustion; Contact with water, carbon dioxide spontaneous combustion; Heat, flame flammable |
| storage and transportation characteristics | The warehouse is ventilated and dried at low temperature; Waterproof, carbon dioxide resistant |
| extinguishing agent | dry powder |
Last Update：2024-04-10 22:29:15
LITHIUM-1-BUTANIDE - Preparation
under the protection of argon, add 3L n-hexane (or 60-90 ℃ petroleum ether) into a 5000ml three-mouth bottle, wash 140g(20mol) metal lithium sheet with n-hexane (or 60-90 ℃ petroleum ether), put on disposable gloves, quickly tear the metal lithium sheet into small pieces, add it into a 5000ml three-mouth bottle, add it to a mechanical stirring, and cool it to about 0, otherwise, the initiation is relatively slow), add 925g(10mol) of chlorobutane dropwise to it, and control the temperature below 15 degrees (note that the reaction is purple gray after initiation, the dropwise addition should be slow at the beginning, the reaction exotherm is relatively severe, and special attention should be paid to not flushing). After adding, the ice salt bath is controlled below 15 degrees to continue stirring for 2 hours, then the ice salt, gradually raise the temperature and reflux for 4-5 hours, cool to room temperature, settle overnight, the supernatant is butyl lithium solution, press into the storage bottle with argon, add 2L solvent to the residue, stir, settle overnight, and merge the supernatant into butyl lithium solution for standby.
Residue treatment: put the upper residue bottle in a basin filled with sand and soil, place it in a safe place, and expose it to the air for 1-2 months (without spontaneous combustion). when the solid in the system turns white, it will come out immediately and splash water on the open space. If the local climate is humid, dry tubes should be added to the bottle mouth on both sides for the first few days. If the reaction bottle is used urgently, after the n-butyl lithium solution is transferred, it can be cooled in an ice salt bath under the protection of argon, and the tert-butanol is slowly added dropwise.
Last Update：2024-04-10 22:29:15
LITHIUM-1-BUTANIDE - Titration and Calibration Methods
butyl lithium must be calibrated before use. double titration is complicated and generally not used. single titration can be used. The specific method is as follows:
1) Titration reagent: 1mol/L sec-butanol/xylene solution (both sec-butanol and xylene must be dried with activated 5A molecular sieve)
2) indicator: 2,2 '-bipyridine
3) solvent: xylene (must be dried with activated 5A molecular sieve)
4) Operation method: Under the protection of argon, add magnetons, 20ml xylene, and a small amount of indicator to a 100ml three-mouth bottle with a flip plug, and then use a 2ml syringe with a precise scale to accurately measure 2ml butyl lithium and quickly transfer it to the bottle (the air in the syringe needs to be replaced by argon, and the argon in the syringe needs to be removed when extracting butyl lithium, and the argon in the syringe needs, in order to prevent the trace amount of water and air in the syringe from affecting the accuracy of titration), the system becomes purplish red, and then the same syringe (the purpose of using the same syringe is to reduce the titration error) is cleaned, dried, washed two to three times with titrant, and the titrant titration system is changed to yellow accurately, which is the titration end point.
5) If the titration is repeated once and the error between the two times is within 2%, the result can be considered accurate.
6) Titration result: titration dose (ml)/2 is the molar concentration of butyl lithium
Note:
1) n-butyl lithium is very easy to ignite spontaneously when exposed to air. when measured, the tip of the needle will emit sparks in the air.
2) Argon must be used for protection during the whole process, and special attention should be paid to safety.
3) When butyl lithium catches fire, sand shall be used to extinguish the fire. Sand for fire fighting must be provided within reach.
4) When preparing and using butyl lithium, it is best not to operate it alone, so as not to be handled by one person in case of accidents.
Last Update：2024-04-10 22:29:15
LITHIUM-1-BUTANIDE - Precautions for Use
n-butyl lithium is a multi-purpose anionic polymerization initiator. In recent years, explosions and fires caused by butyl lithium have been reported frequently. So how can we avoid these tragedies as much as possible in the experiments using butyl lithium?
(1) Butyllithium is very easy to ignite spontaneously when exposed to air. When measuring, the tip of the needle will emit sparks in the air;
(2) The whole process must be protected with inert gas, and special attention should be paid to safety;
(3) When butyl lithium catches fire, sand shall be used to extinguish the fire. Usually there must be sand for fire fighting within reach;
(4) When preparing and using butyl lithium, it is best not to operate it alone, so as not to be able to handle it alone in case of accidents;
(5) n-butyl lithium is a reagent with strong nucleophilicity and can initiate anionic polymerization. Plastic or rubber containers should be avoided and stored at low temperature without light and water.
(6) The reaction system and solvent using butyl lithium should be strictly anhydrous and oxygen-free;
(7) Butyl lithium should not be stained or dripped on flammable substances (such as acetone cold bath in Dewar);
(8) In the process of taking butyl lithium, the needle will be blocked (solid or rubber scraps with reverse plug in front of the needle are stuffed into the needle hole when the air humidity is high). It is necessary to be calm and tell the person accompanying you to operate to handle it properly in time.
(9) Once butyl lithium drips onto the table or the ground, do not be nervous and cover it with asbestos cloth or sand immediately. Never drip into clothes or solvents;
(10) When the dosage is large, it is recommended to directly use a dry and clean stainless steel catheter, and slowly drop butyl lithium into the reaction system through the tiny positive pressure of a suitable inert gas that can control the flow rate. The measure to interrupt at any time is to timely pump the stainless steel catheter from below the butyl lithium liquid level to above the liquid level.
(11) The addition speed of butyl lithium should be strictly controlled. If the weather humidity is slightly higher, the outer wall of the frozen bottle exposed above the surface of dry ice-acetone bath will form thick frost, and it is basically impossible to clearly observe the reaction speed in the reaction bottle.
Last Update：2024-04-10 22:29:15
LITHIUM-1-BUTANIDE - Use
- polymerization catalyst, hydrocarbon agent.
- Used as an intermediate and linking agent for chemical products
- Butyllithium is very widely used in organic synthesis, increasing carbon chain, and is a relatively basic laboratory product. 1. Metallization reaction: R-H n-Butyl-Li & rarr; R-Li Butane, the resulting substance alkyl lithium can react with various substances. 2. Direct metallization reaction: the aromatic compound connecting the substituent reacts with n-butyl lithium, and the metallic lithium can be connected to the aromatic compound. 3. Nucleophilic addition and substitution reaction 4. Halogen-metal replacement
- n-butyl lithium solution is mainly used as anionic polymerization initiator in organic reaction synthesis of pharmaceutical intermediates, and is also used in synthetic rubber, flavor synthesis, liquid crystal materials and other industries and fields.
- n-butyl lithium (n-C4H9Li) is mainly used as organic reaction catalyst, which is widely used in organic catalytic reactions of pharmaceutical intermediates, liquid crystal monomers, pesticides and rubber industries.
Last Update：2024-04-10 22:41:56
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