Recrystallization process of flutamide

A flutamide and recrystallization technology, which is applied in the field of flutamide recrystallization technology, can solve the problems of no more than 0.0002%, benzene or toluene cannot be used continuously, and a large amount of solvent is used, so as to reduce harmful components and other Solvent loss, effect of reducing production cost

Inactive Publication Date: 2013-11-27
KUNSHAN SANYOU PHARMA MATERIAL
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The operation is cumbersome, the amount of solvent used is large, and the cost is high
According to the provisions of (Appendix VIII P Residual Solvent Determination Method of Chinese Pharmacopoeia II,

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A recrystallization process of flutamide, comprising the following steps: in a 500mml three-necked flask equipped with a stirrer, a thermometer, and a dropping funnel, add 300mml of medicinal ethanol, add 100g of flutamide crude product and 5g of activated carbon under stirring, and heat Stir and reflux for 15 minutes, filter while hot to remove activated carbon. Put the liquid in an 800mm beaker and stir, slowly add about 120mml of distilled water into the beaker with a dropping funnel at room temperature, stop adding water when it is slightly mixed, and then use a dropper to drop a few drops of ethanol into the beaker until it becomes clear. Seal and refrigerate to about 5°C, take it out, add about 0.2g of 99.5% flutamide seed crystals to it, gradually observe that yellowish needle-like crystals slowly precipitate out, and gently stir it with a clean glass rod for a few times. Then continue to refrigerate at 0°C for 3 hours. Slip crystals, dry at 60°C for 8 hours, me...

Embodiment 2

[0025] A recrystallization process of flutamide, comprising the following steps: in a 500mml three-necked flask equipped with a stirrer, a thermometer, and a dropping funnel, add 80mml of medicinal ethanol and 120mml of petroleum ether, and add 80g of crude product of flutamide under stirring ( Moisture content below 3%), activated carbon 4g, heated and stirred under reflux for 15 minutes, filtered while hot to remove the activated carbon. Add the slip liquid into another 500mml three-necked flask equipped with a stirrer, a thermometer, and a dropping funnel, stir and raise the temperature to 50°C, slowly add about 70mml of petroleum ether through the dropping funnel, and stop adding petroleum ether until it is slightly mixed. Then drop a few drops of petroleum ether into the beaker with a dropper until it becomes clear. Cool to room temperature without oily layering (if there is oily layering, it means that the water content of the crude product is too high), seal and refrige...

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Abstract

The invention discloses a recrystallization process of flutamide. The recrystallization process of the flutamide comprises the following steps: adding medicinal ethanol or medicinal ethanol and petroleum ether into a reaction kettle with a stirring machine, a thermometer and a dropping funnel, adding flutamide crude products and active carbon under stirring, heating, stirring and refluxing, and filtering and distilling to remove active carbon when still hot to obtain distillate; placing the distillate into a beaker, stirring, slowly adding distilled water or petroleum ether into the beaker at a certain temperature by using the dropping funnel, stopping adding the distilled water or the petroleum ether when slightly mixing, and adding ethanol into the beaker dropwise by using a dropper until the solution is clear; performing sealed refrigeration until 3 to 7 DEG C and taking out, adding flutamide seed crystals with the purity being more than 99.3%, separating out yellowish needle-shaped crystals slowly, and slightly stirring for several times by using a clean glass rod; continuously performing refrigeration at 0 DEG C for 3 hours; and distilling to take crystals and drying at 60 DEG C for 8 hours, wherein melting point is 110 to 113 DEG C and purity is more than 99%. Benzene or methylbenzene is replaced by solvents such as ethanol and petroleum ether, so the deadlock that the flutamide is difficult to recrystallize is broken and harmful components of the flutamide products are reduced.

Description

technical field [0001] The invention relates to a recrystallization process of flutamide, which belongs to the technical field of chemical synthesis process. Background technique [0002] At present, there are pharmaceutical manufacturers with GMP certificates in my country. At present, the production route of flutamide is generally adopted: (1) first acylation to produce m-isobutyramide trifluorotoluene; (2) followed by mixed acid of sulfuric acid and nitric acid The crude product of flutamide can be obtained by nitration; the qualified product can be obtained by recrystallization from benzene or toluene. The residual amount of benzene or toluene is generally controlled below 100ppm. According to (Chinese Pharmacopoeia II, 1995 Edition, Appendix VIII P Residual Solvent Determination Method), the residual amount of benzene or toluene should not exceed 0.01%. If benzene or toluene is used for recrystallization, the residual amount should be less than 0.01%. Ethanol or other s...

Claims

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Application Information

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IPC IPC(8): C07C231/24C07C233/15
Inventor 吴小弟
Owner KUNSHAN SANYOU PHARMA MATERIAL
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