1-broMo -2-Ding Que
1-bromo-2-butyne
CAS: 3355-28-0
Molecular Formula: C4H5Br
1-broMo -2-Ding Que - Names and Identifiers
| Name | 1-bromo-2-butyne |
| Synonyms | 1-bromo-2-butyne 1-BROMO-2-BUTYNE 1-bromobut-2-yne 2-BUTYNYL BROMIDE 2-Butyne, 1-bromo- 1-broMo -2-Ding Que But-2-yn-1-yl bromide |
| CAS | 3355-28-0 |
| EINECS | 608-891-3 |
| InChI | InChI=1/C4H5Br/c1-2-3-4-5/h4H2,1H3 |
| InChIKey | LNNXOEHOXSYWLD-UHFFFAOYSA-N |
1-broMo -2-Ding Que - Physico-chemical Properties
| Molecular Formula | C4H5Br |
| Molar Mass | 132.99 |
| Density | 1.519 g/mL at 25 °C (lit.) |
| Boling Point | 40-41 °C/20 mmHg (lit.) |
| Flash Point | 97°F |
| Solubility | Miscible with acetonitrile. |
| Vapor Presure | 15.2mmHg at 25°C |
| Appearance | Liquid |
| Specific Gravity | 1.519 |
| Color | Clear pale yellow-greenish |
| BRN | 605306 |
| Storage Condition | Inert atmosphere,Room Temperature |
| Refractive Index | n20/D 1.508(lit.) |
1-broMo -2-Ding Que - Risk and Safety
| Risk Codes | 10 - Flammable |
| Safety Description | S16 - Keep away from sources of ignition. S24/25 - Avoid contact with skin and eyes. |
| UN IDs | UN 1993 3/PG 3 |
| WGK Germany | 3 |
| FLUKA BRAND F CODES | 10-23 |
| HS Code | 29033990 |
| Hazard Class | 3 |
| Packing Group | III |
1-broMo -2-Ding Que - Reference Information
| background | 1-bromo-2-butyne is commonly used to synthesize axial chiral ternary compounds. the production of 1-bromo-2-butyne mainly adopts a two-step method, that is, 2-butyne-1-ol is prepared first, and then 2-butyne-1-ol is brominated by bromine process. this scheme has the following disadvantages. |
| Uses | 1-bromo-2-butyne is a light yellow to yellow liquid, mainly used as a lilaglidine intermediate. 1-bromo-2-butyne organic synthesis intermediates and pharmaceutical intermediates, commonly used to synthesize axial chiral ternary compounds, can be used in laboratory research and development process and chemical production process is mainly used as liraglidine intermediates. Liragliptin intermediate |
| application | 1-bromo-2-butyne is an organic synthesis intermediate and a pharmaceutical intermediate, which can be used in laboratory research and development processes and chemical production processes. |
| Preparation | A production method of 1-bromo-2-butyne, which is characterized in that 2-butyn-1-ol is brominated with phosphorus tribromide. The reaction principle is: The preparation method of 2-butyn-1-ol is: first react bromoethane with metal magnesium in THF to prepare Grignard reagent, then add paraformaldehyde to the Grignard reagent for the format reaction. After the format reaction is over, 2-butyne-1-ol is separated and recovered. First, 2-butyne-1-ol is mixed with organic solvent and pyridine, and then dropwise Add phosphorus tribromide for bromination reaction, and separate and recover 1-bromo-2-butyne after the bromination reaction. |
| synthesis process | operation 1: check that all equipment is in normal condition. 90kg of magnesium chips are added into a 2000L dry reaction kettle, the reaction kettle is vacuumized, 150kg of THF is pumped into the reaction kettle, and the stirring mechanism in the reaction kettle is started. A small amount of bromoethane is added into the reaction kettle, and the temperature is increased to initiate the reaction. (When the temperature in the reaction kettle rises obviously and the reflux occurs in the return pipe), the remaining 900kgTHF is added into the reaction kettle, and then 360kg of bromoethane is added dropwise to control the temperature in the reaction; after dropping, heat preservation reaction for 2 hours; After the heat preservation is completed, the reaction kettle is cooled to 5 ℃, propyne gas is introduced into the reaction kettle, and the propyne feeding speed is controlled to be 8kg per hour and completed within 10 hours. After propyne feeding, keep the temperature at 5 ℃ for 12 hours; The reaction kettle was heated to 45 ℃, and paraformaldehyde was added in batches (about 3-6kg was added every 15 minutes), totaling 100kg, during the addition process, the reaction temperature shall not exceed 45 ℃. After adding paraformaldehyde, heat preservation reaction is carried out for 3 hours, then the temperature is raised to 55 ℃ for 1 hour, and sampling is carried out for detection. After the reaction is over, the temperature of the reaction kettle is reduced to 20 ℃, and then the reaction droplets in the reaction kettle are added to a 2000L reaction kettle filled with 500kg of water at 5 ℃. After dropping, stop stirring, let stand for 30min, and vacuum draw out the upper liquid phase. After pumping, 10% dilute hydrochloric acid is added to the lower liquid phase, the pH of the system is adjusted to 5 (about), and the upper liquid is left to layer again. The upper liquid is transferred to the transfer tank, the lower liquid is extracted twice with methyl tert-butyl ether, and organic matter is recovered in layers; the organic matter in the transfer tank is combined with the organic matter extracted and recovered from methyl tert-butyl ether, and then the pH of the organic matter is adjusted to 6 with saturated sodium bicarbonate aqueous solution; then Transfer to a 2000L reactor for reduced pressure distillation to recover the solvent THF and methyl tert-butyl ether; the concentrated liquid after reduced pressure distillation is transferred to a 500L rectification tower, and 130kg of fraction (2-butyne -1-alcohol) with purity above 97%; operation 2: 180kg of 2-butyne -1-alcohol, 700kg of methyl tert-butyl ether and 25kg of pyridine are pumped into a 1000L dry reactor. The temperature in the reactor is reduced to -5 ℃; 280kg of phosphorus tribromide is slowly added to the reactor, and the temperature is controlled below 0 ℃ for 10 hours. After the dripping is completed, heat preservation at -5 ℃ for 4 hours and then raise the temperature to 40 ℃ for reaction (GC detects that the raw material reaction is complete); After the reaction is over, the temperature in the reaction kettle is reduced to below 20 degrees, the reaction liquid is transferred to a 2000L reaction kettle filled with 500L of water, the temperature is controlled below 20 degrees, stirred and mixed for 1 hour, and then left to layer; The upper organic phase is recovered, the lower aqueous phase is separated, and the reaction liquid phase is extracted twice with methyl tert-butyl ether, the combined organic phase is washed with water twice, each time with 300kg of water, and the washed organic phase is transferred to a 2000L concentration kettle for decompression concentration; After the concentration is completed, the concentrated liquid is transferred to a 500L rectification kettle, and the distillation is reduced to collect more than 98% fractions to obtain 280kg of product (1-bromo-2-butyne). |
Last Update：2024-04-10 22:29:15
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