LABOTEST-BB LT00771921
diflunisal
CAS: 22494-42-4
Molecular Formula: C13H8F2O3
LABOTEST-BB LT00771921 - Names and Identifiers
| Name | diflunisal |
| Synonyms | diflunisal DIFLUSINAL LABOTEST-BB LT00771921 5-[2,4-DIFLUOROPHENYL]SALICYLIC ACID 5-(2,4-Difluorophenyl) salicylic acid 5-(3,4-difluorophenyl)-2-hydroxy-benzoic acid 2',4'-difluoro-4-hydroxybiphenyl-3-carboxylic acid 2',4'-DIFLUORO-4-HYDROXY-BIPHENYL-3-CARBOXYLIC ACID 1'-biphenyl)-3-carboxylicacid,2',4'-difluoro-4-hydroxy-( 1'-biphenyl]-3-carboxylicacid,2',4'-difluoro-4-hydroxy-[ 2',4'-DIFLUORO-4-HYDROXY[1,1'-BIPHENYL]-3-CARBOXYLIC ACID [1,1'-Biphenyl]-3-carboxylic acid, 2',4'-difluoro-4-hydroxy- |
| CAS | 22494-42-4 |
| EINECS | 245-034-9 |
| InChI | InChI=1/C13H8F2O3/c14-10-3-1-8(6-11(10)15)7-2-4-12(16)9(5-7)13(17)18/h1-6,16H,(H,17,18) |
LABOTEST-BB LT00771921 - Physico-chemical Properties
| Molecular Formula | C13H8F2O3 |
| Molar Mass | 250.2 |
| Density | 1.3505 (estimate) |
| Melting Point | 207-209?C |
| Boling Point | 386.9±42.0 °C(Predicted) |
| Flash Point | 198.7°C |
| Water Solubility | 6.186mg/L(24.99 ºC) |
| Solubility | Practically insoluble in water, soluble in ethanol (96 per cent). It dissolves in dilute solutions of alkali hydroxides. |
| Vapor Presure | 2.75E-07mmHg at 25°C |
| Appearance | White solid |
| Color | White |
| pKa | pKa 3.3 (H2O I=0.1) (Uncertain) |
| Storage Condition | Keep in dark place,Sealed in dry,Room Temperature |
| Refractive Index | 1.601 |
| Physical and Chemical Properties | Crystals. Melting Point 210-211 ° C, difficult to dissolve in water. |
| Use | Mainly used for the treatment of rheumatoid arthritis and rheumatoid arthritis, back, shoulder, knee, neck strain or sprain and tumor caused by postoperative pain |
LABOTEST-BB LT00771921 - Risk and Safety
| Risk Codes | R22 - Harmful if swallowed R36/37/38 - Irritating to eyes, respiratory system and skin. R63 - Possible risk of harm to the unborn child |
| Safety Description | S22 - Do not breathe dust. S26 - In case of contact with eyes, rinse immediately with plenty of water and seek medical advice. S36 - Wear suitable protective clothing. |
| WGK Germany | 3 |
| RTECS | DV2030000 |
| HS Code | 2918290000 |
| Hazard Note | Irritant |
| Toxicity | LD50 orally in female mice: 439 mg/kg (Stone) |
LABOTEST-BB LT00771921 - Standard
Authoritative Data Verified Data
This product is difluoro-4-hydroxy-3-biphenyl carboxylic acid, calculated as dry product, containing no less than 98.5% of c13h23-203.
Last Update：2024-01-02 23:10:35
LABOTEST-BB LT00771921 - Trait
Authoritative Data Verified Data
- This product is white or off-white crystalline or crystalline powder; Odorless.
- This product is soluble in methanol, soluble in ethanol; Slightly soluble in chloroform; Almost insoluble in water.
Last Update：2022-01-01 11:29:45
LABOTEST-BB LT00771921 - Differential diagnosis
Authoritative Data Verified Data
- take about 2mg of this product, add 10ml of ethanol to dissolve, add 1 drop of ferric chloride test solution, that is, deep purple.
- take this product, add 0.1 mol/L hydrochloric acid in ethanol solution dissolved and diluted to prepare solution containing 20ug per 1 ml, according to UV-visible spectrophotometry (General 0401) determination, there is a maximum absorption at the wavelength of 251nm and 315nm, and the absorbance ratio should be 4.2 to 4.6.
- The infrared absorption spectrum of this product should be consistent with that of the control (Spectrum set 901).
Last Update：2022-01-01 11:29:46
LABOTEST-BB LT00771921 - Exam
Authoritative Data Verified Data
Related substances I
take this product, add methanol to dissolve and dilute to make a solution containing about 10mg per lml, as a test solution; Take an appropriate amount of precision, A solution containing about 50ug per 1 ml, which is prepared by quantitative dilution with methanol, is used as a control solution, and 5ul of each of the above two solutions is absorbed according to the thin layer chromatography method (General 0502), respectively, with n-hexane-Dioxane-glacial acetic acid (85:10:5) as the developing solvent, on the same silica gel GF254 thin layer plate, expand, dry, and set the UV lamp (254nm) for inspection, test solution such as impurity spots, compared with the control solution of the main spot, not deeper.
Related substances II
The Test Solution and the control solution under the item of related substances 1 were taken and tested by high performance liquid chromatography (General 0512). Silica gel bonded with eighteen alkyl silane was used as filler; Water-methanol-acetonitrile-glacial acetic acid (55:23:30:2) was used as mobile phase; The detection wavelength was 254nm. The number of theoretical plates shall not be less than 2000 based on the calculation of the peak of diflmenstrual. 5 u1 of each of the control solution and the test solution under item I of related substances are accurately measured and injected into the human liquid chromatograph respectively, and the chromatogram is recorded to 3 times of the retention time of the main component peak. If there are impurity peaks in the chromatogram of the test solution, the sum of each impurity peak area shall not be greater than the main peak area of the control solution (0.5%).
loss on drying
take this product, with pentoxide as desiccant, at 60°C under reduced pressure drying to constant weight, loss of weight shall not exceed 0.3% (General rule 0831).
fluorine content
take this product about 13mg, precision weighing, according to the fluorine inspection method (General 0805) determination, according to the dry product calculation, fluorine content should be 14.5% ~ 15.5%.
ignition residue
take l.Og of this product and check it according to law (General rule 0841). The residue left shall not exceed 0.1%.
Heavy metals
The residue left under the item of taking the ignition residue shall not contain more than 10 parts per million of heavy metal when examined by law (General Principles 0821, Law II).
Last Update：2022-01-01 11:29:47
LABOTEST-BB LT00771921 - Content determination
Authoritative Data Verified Data
take this product about 0.45g, precision weighing, add methanol 80ml to dissolve, add water 10ml and phenol red indicator solution (take red 0.lg, add 0.2mol/L sodium hydroxide solution 1.4ml, 90% ethanol 5ml, slightly warm to dissolve, diluted with 20% ethanol to ML, obtained) 8~10 drops, with sodium hydroxide titration solution (0.1 mol/L) titration, and the results of the titration were corrected with a blank test. Each 1 ml of sodium hydroxide titration solution (0.1 mol/L) corresponds to 25.02mg of c13hfp203.
Last Update：2022-01-01 11:29:47
LABOTEST-BB LT00771921 - Category
Authoritative Data Verified Data
antipyretic analgesic, non-steroidal anti-inflammatory drugs.
Last Update：2022-01-01 11:29:47
LABOTEST-BB LT00771921 - Storage
Authoritative Data Verified Data
light shielding, sealed storage.
Last Update：2022-01-01 11:29:48
LABOTEST-BB LT00771921 - Diflunix tablets
Authoritative Data Verified Data
This product contains diflcouple (c11hfp203) should be the label amount of 95.0% ~ 105.0%.
trait
This product is a film-coated tablet, white or off-white after removal of the coating.
identification
- take an appropriate amount of fine powder of this product (about 2mg of difloup), add 10ml of ethanol, shake to dissolve difloup, and add 1 drop of ferric chloride test solution, which shows a deep purple color.
- 2ml of the test solution under the item of related substances was diluted to 50ml with acetonitrile-water (4:1) as the test solution, and an appropriate amount of the reference substance of diflunix was taken, acetonitrile-water (4:1) was added and dissolved and diluted to prepare a solution containing about 40mg per 1 ml as a control solution. The chromatogram shall be recorded according to the chromatographic condition test under the item of related substances. The retention time of the main peak of the test solution should be consistent with the retention time of the main peak of the control solution.
- take the test solution under the content determination item and use 0.1 mol/L hydrochloric acid ethanol solution was diluted to prepare a solution containing about 20ug of difloniclovir per 1 ml, and the maximum absorption was measured by UV-visible spectrophotometry (General 0401) at the wavelength of 251nm and 315nm.
examination
- Related Substances: take an appropriate amount of this product's fine powder, add acetonitrile-water (4:1) to dissolve and dilute to make about 1 diflunix in each lml. 0 mg of the solution, filtered, and the filtrate was taken as the test solution. Take 1 ml of the solution, put it in a 200ml measuring flask, dilute it to the scale with acetonitrile-water (4:1), and shake it well, as a control solution. According to the high performance liquid chromatography (General 0512) test, silica gel bonded with eighteen alkyl silane was used as filler; Water-methanol-acetonitrile-glacial acetic acid (55:25:70:2) was used as mobile phase; the detection wavelength was 254mn. The number of theoretical plates shall not be less than 2000 based on the calculation of the peak of diflmenstrual. Take 10ul of the control solution and the sample solution respectively, inject the human liquid chromatograph, record the chromatogram to 3 times the retention time of the main component peak. If there are impurity peaks in the chromatogram of the test solution, the sum of each impurity peak area shall not be greater than that of the control solution.
- peak area (0.5%).
- dissolution of this product, according to the dissolution and release determination method (General 0931 second method), with 0.1 mol/L Tris buffer solution (25% G of Tris was weighed, dissolved in water and diluted to 7.2 mL, adjusted to pH with citric acid solution and diluted to 10 000mL with water) was used as dissolution medium, the rotation speed is 50 revolutions per minute, and the operation is carried out according to law. After 30 minutes, 10ml of the solution is taken, filtered, and the appropriate amount of the filtrate is taken, the solution containing about 30 tons per lml is prepared by quantitative dilution with dissolution medium as the test solution. In addition, an appropriate amount of the reference substance of diflmenstrual is is taken, the dissolution medium was added to dissolve and quantitatively dilute to prepare a solution containing about 30ug per 1 ml as a control solution. The absorbance of each of the above two Solutions was measured at a wavelength of 306mn by ultraviolet-visible spectrophotometry (General 0401), and the elution amount of each tablet was calculated. The limit is 80% of the labeled amount and shall be in accordance with the provisions.
- others shall be in accordance with the relevant provisions under the item of tablets (General rule 0101).
Content determination
Take 20 tablets of this product, precision weighing, fine grinding, precision weighing an appropriate amount (about 0.lg equivalent to diflunix), put it in a 100ml measuring flask, add 0.1 mol/L hydrochloric acid and ethanol solution, ultrasonic dissolution of diflunix, cool, with 0. Dilute 1 mol/L hydrochloric acid ethanol solution to the scale, shake well, filter, Take 5ml of continuous filtrate accurately, put it in a 100ml measuring flask, use 0.1 mol/L hydrochloric acid ethanol solution diluted to the scale, shake, as a test solution, according to UV-visible spectrophotometry (General 0401), at the wavelength of 315mn absorbance; take an appropriate amount of the reference product of diflunix and weigh it precisely, add 0.1 mol/L hydrochloric acid fermentation solution was dissolved and quantitatively diluted to prepare a solution containing about 50 Mixes per 1 ml, which was used as a reference solution and measured by the same method. It is obtained by calculation.
category
Same as diflunix.
specification
0.25g
storage
sealed storage.
Last Update：2022-01-01 11:29:49
LABOTEST-BB LT00771921 - Diflunix capsules
Authoritative Data Verified Data
This product contains diflcouple (c1h23-203) should be the label amount of 90.0% ~ 110.0%.
trait
The content of this product is white or white fine particles.
identification
- take an appropriate amount of the content of this product (about 2mg equivalent to diflunix), add 10ml of ethanol, shake, and add 1 drop of ferric chloride test solution, which shows a deep purple color.
- take the solution under the content determination item and use 0. Dilute 1 mol /L hydrochloric acid in ethanol solution to prepare a solution containing about 20PG of difloniclovir per 1 ml, and determine by UV-Vis spectrophotometry (General 0401), there is a maximum absorption at the wavelength of 251nm and 315nm.
- take an appropriate amount of the content of this product (about 50mg equivalent to difloniclovir), add 5ml of methanol, shake to dissolve difloniclovir, filter, filtrate as a test solution; in addition, taking an appropriate amount of the reference substance of difloniclovir and dissolving it with methanol to make a solution containing about 10mg per 1 ml, which is used as the reference solution and tested by thin layer chromatography (General rule 0502), draw 5 u1 of each of the above two solutions, respectively, on the same silica gel GF2S4 thin layer plate, with n-hexane-Dioxane-glacial acetic acid (85:10:5) as the developing agent, spread out and dry, check under ultraviolet light (254nm), the position and color of the main spot of the test solution should be consistent with the main spot of the reference solution.
examination
- dissolution of this product, according to the dissolution and release determination method (General 0931 second method), with 0.1 mol/L Tris buffer solution (25% G of Tris was weighed, dissolved in water and diluted to 7.2 mL, adjusted to pH with citric acid solution and diluted to 10 000mL with water) was used as dissolution medium, the rotation speed is 50 revolutions per minute, and the operation is carried out according to law. After 30 minutes, 10ml of the solution is taken, filtered, and the appropriate amount of the filtrate is taken, dilute with dissolution medium to prepare a solution containing about 30ug per lml as a test solution; Take an appropriate amount of diflorixan reference substance and weigh it precisely, the dissolution medium was added to dissolve and quantitatively dilute to prepare a solution containing about 30ug per 1 ml as a control solution. The absorbance of each of the above two Solutions was measured at a wavelength of 0401 nm by ultraviolet-visible spectrophotometry (general), and the elution amount of each particle was calculated. The limit is 80% of the labeled amount and shall be in accordance with the provisions.
- others should comply with the relevant provisions under the capsule (General 0103).
Halo-containing assay
take the content under the item of difference in loading, grind it, weigh it accurately, take an appropriate amount (about 0.lg equivalent to diflonix), put it in a 100ml measuring flask, add 0.1 mol/L hydrochloric acid and ethanol solution, ultrasonic dissolution of diflunix, cool, with 0. Dilute 1 mol/L hydrochloric acid ethanol solution to the scale, shake well, filter, Take 5ml of continuous filtrate accurately, put it in a 100ml measuring flask, use 0. Dilute the lmol/L hydrochloric acid ethanol solution to the scale, shake well, measure the absorbance at the wavelength of 315nm by UV-Vis spectrophotometry (General rule 0401 ), precision weighing, add 0.1 mol/L hydrochloric acid ethanol solution was dissolved and quantitatively diluted to prepare a solution containing about 50 WW per 1m l as a reference solution, which was determined by the same method. It is obtained by calculation.
category
Same as diflunix.
specification
0.25g
storage
sealed storage.
Last Update：2022-01-01 11:29:50
LABOTEST-BB LT00771921 - Reference Information
| NIST chemical information | Information provided by: webbook.nist.gov (external link) |
| overview | diflunisal (diflunisal), a non-steroidal anti-inflammatory analgesic, is the most promising alternative to aspirin. It is clinically used to treat rheumatoid arthritis, rheumatoid arthritis, osteoarthritis, sprain, strain and analgesia. Studies have shown that diflunisal and ibuprofen have considerable efficacy in the treatment of rheumatoid arthritis and degenerative arthritis. The observation also found that diflunisal is significantly better than ibuprofen in improving the grip strength of patients with rheumatoid arthritis and relieving arthralgia and tenderness of rheumatoid arthritis and degenerative arthritis. At the same time, diflunisal has a decreasing and relieving effect on rheumatoid factor titer and morning stiffness in patients with rheumatoid arthritis. The analgesic effect of diflunisal is 7.5 to 13 times that of aspirin, and the antipyretic effect is 1.4 times that of aspirin. Times, its therapeutic effect is about 3 times that of aspirin, so it is suitable for the treatment of rheumatoid arthritis, osteoarthritis, muscle sprain, strain, meniscus surgery, orthopedic surgery and oral surgery, and primary dysmenorrhea. Moderate pain is worthy of clinical application. Diflunisal was selected from more than 500 salicylic acid derivatives by Merck Sharp & Do hme Company in the United States with flunisal (flunisal) as the lead compound and was listed in 1975. At present, Merck is one of the varieties with annual sales of more than 0.1 billion US dollars, and has been listed in more than 70 countries such as Britain, the United States, Japan, Italy and France. The previous versions of the United States Pharmacopoeia and the British Pharmacopoeia have been included. China has approved the production of diflunisal tablets and diflunisal capsules. |
| pharmacokinetics | this product is well absorbed by oral administration. the blood drug concentration reaches a peak 2~3h after taking it. the half-life is proportional to the dosage of the drug, about 8~12h, and the plasma protein binding rate is 90%. Oral 125mg, 3~4 days, 500mg for 7~9 days. The elimination half-life is 7~8h for 125mg and 15h for 500mg. The binding rate with plasma protein is as high as 98% ~ 99% in normal people. The milk content of lactating women is 2% ~ 7% of the blood drug concentration, which is not metabolized into salicylic acid in the body. 80% ~ 95% drugs are excreted from urine in 72~96h with two soluble glucuronide conjugates. |
| Synthetic route | 4-(2',4'-difluorophenyl) phenol is synthesized into diflunisal by Kolbe-Schmitt carboxylation. Operation steps: add KHCO3 and 4-(2 ',4'-difluorophenyl) phenol 0.5g(2.43mmol) into the reaction bottle, mix evenly, then pass into CO2, place in a microwave reactor (220W), and react at the set temperature for a certain period of time under stirring. Cool to 80 ℃, filter, dissolve the filter cake with boiling water, filter while hot, wash the filter cake with a small amount of boiling water, combine the filtrate and washing liquid, adjust to pH7 with dilute hydrochloric acid, cool to room temperature, extract with trichloroethylene (3 × 20mL), heat and clarify the water layer, adjust with dilute hydrochloric acid to pH2, cool to room temperature, precipitate, filter, wash the filter cake with ice water to neutral, vacuum drying at 70 ℃ for 8h to obtain white solid diflunisal. Fig. 1 shows the synthesis route of diflunisal |
| clinical application | this product can inhibit the synthesis of prostaglandins and exert analgesic, anti-inflammatory and antipyretic effects. It is used for analgesia of mild and moderate pain of bone and rheumatoid arthritis, and also for pain relief after meniscus and orthopedic surgery, as well as joint and muscle sprain and cancer pain. It is effective for 1 hour and can last for 8~12 hours. It can also be used for osteoarthritis, rheumatoid arthritis, etc. (2016-01-22) |
| precautions | 1. combination with hydrochlorothiazide, indomethacin and acetaminophen can increase the plasma concentration of these drugs. 2. Long-term application can cause renal damage and drug accumulation, so patients with renal insufficiency should reduce the amount with caution. 3. Cardiac insufficiency, hypertension, edema, peptic ulcer and bleeding are prohibited, and pregnant and lactating women are prohibited. 4. Those who are allergic to this product and acetylsalicylic acid are prohibited. 5. Take it together with anticoagulant, which can prolong coagulation time. |
| adverse reactions | 1. digestive system: loss of appetite, nausea, abdominal pain, abdominal distension, diarrhea and constipation, etc. 2. Nervous system: dizziness, headache, fatigue, insomnia, lethargy, etc. 3. Others: occasional rash, edema, rhinitis, tinnitus, transient visual impairment, etc. |
| usage and dosage | for different symptoms, the dosage of this product is different. 1. Analgesia: start taking 1g, and then 0.5g every 8~12h. 2. Osteoarthritis: 0.5~1g per day, taken in divided doses, and the maintenance amount shall not exceed 1.5g for 1d. |
| use | antipyretic analgesic, suitable for mild to moderate pain. It is also a medication for the digestive system. It is mainly used to treat rheumatoid arthritis and rheumatoid arthritis, back, shoulder, knee, neck strain or sprain, and pain caused by tumor surgery |
| production method | 4-(2 ',4'-difluorophenyl) phenol can be prepared by carboxylation of carbon dioxide. The intermediate 4-(2 ',4'-difluoroaniline) phenol was synthesized according to the following route. |
Last Update：2024-04-10 22:29:15
Supplier List
Spot supply
Product Name: Diflunisal Visit Supplier Webpage Request for quotationCAS: 22494-42-4
Tel: 18301782025
Email: 3008007409@qq.com
Mobile: 18021002903
QQ: 3008007409
Wechat: 18301782025
Spot supply
Product Name: Diflunisal Visit Supplier Webpage Request for quotationCAS: 22494-42-4
Tel: 18301782025
Email: 3008007409@qq.com
Mobile: 18021002903
QQ: 3008007409
Wechat: 18301782025
View History