Process for synthesizing flutamide

A synthesis process and flutamide technology, applied in the field of flutamide synthesis technology, can solve the problems of complex recrystallization, difficult quality control, complex production process and the like, and achieve high catalyst activity, few impurities and low production cost. Effect

Inactive Publication Date: 2015-05-20
KUNSHAN SANYOU PHARMA MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Compared with each other, there are advantages and disadvantages: the advantage of route (1) is that there are fewer production processes; the disadvantage is that recrystallization is more complicated and the quality is not easy to control
The advantage of route (2) is that recrystallization is simple and the product quality is good; the disadvantage is that the production process is more complicated

Method used

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  • Process for synthesizing flutamide
  • Process for synthesizing flutamide
  • Process for synthesizing flutamide

Examples

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Embodiment 1

[0030] A kind of synthetic technique of flutamide, comprises the following steps:

[0031] a) In a 250mml reaction flask equipped with a stirrer, a thermometer, a dropping funnel and a reflux dehydration device, add 40mml of 1,2-dichloroethane and 10mml of N,N-dimethylacetamide, and add them under stirring 20g of 2-nitro-5-aminotrifluorotoluene and 1.46g of 4-dimethylaminopyridine, slowly add 12.2g of isobutyryl chloride dropwise under ice-water bath conditions at a controlled temperature of 5-10°C, the yellow solution gradually becomes cloudy, and the dropwise addition is completed , remove the ice-water bath, keep the temperature at 18-25°C and stir for a period of time, take samples and monitor the reaction by TLC until the reaction of 2-nitro-5-aminotrifluorotoluene is completely completed;

[0032] b) Change the oil bath, add 60mml of water into the reaction flask, stir to raise the temperature, control the temperature of the oil bath to 105-120°C, reflux to remove the 1,...

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Abstract

The invention discloses a process for synthesizing flutamide. The process comprises the steps of taking 2-nitro-5-aminobenzotrifluoride as a raw material, selecting 1,2-dichloroethane as a solvent and N,N-dimethyl acetamide as an acid absorbent, dropwise adding isobutyryl chloride under the action of 4-dimethylamino pyridine while maintaining the temperature to be 5-10 DEG C, and reacting after the dropwise adding process is completed while maintaining the temperature to be 18-25 DEG C until 2-nitro-5-aminobenzotrifluoride reacts completely; adding water, heating to steam out 1,2-dichloroethane, carrying out elutriation, and filtering to obtain a flutamide crude product; and re-crystallizing by using ethanol, thereby obtaining a flutamide finished product. The process has the advantages of simplicity, few steps, easiness in operation, low cost and high product quality; the conversion ratio of the product is high and reaches over 96%; the activity of a catalyst is high, and side reactions are few; the reaction conditions are mild, and the reaction time is short; the purity of the product is high, and the impurities are few; the production cost is low, and the solvent 1,2-dichloroethane can be repeatedly used indiscriminately; and waste gases, waste water and waste residues are few, thus the environmental friendliness is facilitated.

Description

technical field [0001] The invention relates to a synthesis technique of flutamide, which belongs to the technical field of chemical synthesis techniques. Background technique [0002] There are many synthetic routes for flutamide, and there are two typical production methods. (1) Acylation first and then nitration; (2) First nitration and then acylation. Compared with each other, there are advantages and disadvantages: the advantage of route (1) is that the production process is less; the disadvantage is that the recrystallization is more complicated and the quality is not easy to control. The advantage of route (2) is simple recrystallization and good product quality; the disadvantage is that the production process is more complicated. Contents of the invention [0003] Objective: In order to overcome the deficiencies in the prior art, the present invention provides a synthesis process of flutamide. [0004] Technical solution: In order to solve the above-mentioned te...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/15C07C231/02
Inventor 吴小弟
Owner KUNSHAN SANYOU PHARMA MATERIAL
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