Synthetic method of medicine for treating leprosy

A technology for treating drugs and leprosy, which is applied in the field of medicine, and can solve problems such as long process routes, heavy environmental pollution, and low yields

Active Publication Date: 2013-01-09
CHANGZHOU PHARMA FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This improved process overcomes the shortcomings of low yield, long process route, and large environmental pollution in the prior art, and at the same time solves the problems of solvent residue and solvent recovery and reuse in the refining process

Method used

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  • Synthetic method of medicine for treating leprosy
  • Synthetic method of medicine for treating leprosy
  • Synthetic method of medicine for treating leprosy

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Pump 100kg of N, N-dimethylformamide into the reactor, add 50kg of glutamic acid and 50kg of phthalic anhydride under stirring, then heat, react at 95-100°C for 3 hours, and then distill out N , N-dimethylformamide, cooling and adding 100kg of acetic anhydride, heating to 105-110°C for 1 hour reaction, decompressing to remove excess anhydride, heating the reaction to 230°C, slowly feeding ammonia gas under stirring, and reacting After that, discharge the material while it is hot, put it into a reaction pot with 300kg of water in advance, cool to room temperature, and filter to obtain the crude thalidomide, put the crude thalidomide into a tank with 300L dimethyl sulfoxide In the refining pot, add activated carbon, reflux for 1 hour, filter into the crystallization pot, cool to room temperature, filter, and dry to obtain 70.2 kg of thalidomide finished product, with a yield of 80.6%, a melting point of 274-279°C, and a purity of 99.8%. 1 HNMR (DMSO-d 6 ): 11.12(s, 1H), ...

Embodiment 2

[0022] Draw 100kg of N-methylpyrrolidone into the reactor, add 50kg of glutamic acid and 50kg of phthalic anhydride under stirring, then heat, react at 125-130°C for 1 hour, and then distill out N-methylpyrrolidone under reduced pressure , add 100kg of acetic anhydride after cooling, heat to 80-85°C to react for 3 hours, evaporate the excess anhydride under reduced pressure, heat the reaction to 180°C, slowly feed ammonia gas under stirring, and monitor the reaction by thin-layer chromatography. Discharge the material while it is hot, put it into a reaction pot with 300kg of water in advance, cool to room temperature, filter to obtain the crude thalidomide, put the crude thalidomide into the refining pot with 300L dimethyl sulfoxide , add activated carbon, reflux for 1 hour, filter into a crystallization pot, cool to room temperature, filter, and dry to obtain 72.5 kg of thalidomide finished product, with a yield of 83.2%, a melting point of 274-275°C, and a purity of 99.8%.

Embodiment 3

[0024] Pump 100kg of N, N-dimethylformamide into the reactor, add 50kg of glutamic acid and 50kg of phthalic anhydride under stirring, then heat, react at 80-85°C for 5 hours, and then distill out N , N-dimethylformamide, cooling and adding 100kg of acetic anhydride, heating to 115-120 ° C for 1 hour, decompression to remove excess anhydride, heating the reaction to 230 ° C, and slowly feeding ammonia gas under stirring, the reaction After completion, discharge the material while it is hot, put it into a reaction pot with 300kg of water in advance, cool to room temperature, filter to obtain the crude thalidomide, put the crude thalidomide into a refining pot with 300L of isopropanol Inside, add activated carbon, reflux for 1 hour, filter into a crystallization pot, cool to room temperature, filter, and dry to obtain 75.1 kg of thalidomide finished product, with a yield of 86.2%, a melting point of 273-275°C, and a purity of 99.6%.

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Abstract

The invention belongs to the technical field of medicine and particularly relates to a synthetic method of the medicine for treating leprosy. The synthetic method is characterized in that phthalic anhydride and glutamic acid are used as raw materials, one-pot operation is performed, direct synthesis is performed, and then a finished product is obtained after purification. Yield is improved from 50% to about 80%. Simultaneously, N, N-dimethylformamide and other solvents are adopted in a condensation step. Compared with a solvent pyridine used in the original process, environment pollution is reduced, and cost is saved. Dimethyl sulfoxide is used as a solvent during purification, and purified mother liquor is recycled. Compared with the solvent N, N-dimethylformamide adopted by the original process, the low-toxicity solvent is used, the problem that the original process is much in impurities and unqualified in residual solvent is solved, and the purified mother liquor is recycled so as to reduce product cost further.

Description

Technical field: [0001] The invention belongs to the technical field of medicine, and in particular relates to a method for synthesizing leprosy medicine thalidomide. Background technique: [0002] Thalidomide (Thalidomide) alias: reaction stopper, thalidomide, its structural formula is as follows: [0003] [0004] Thalidomide was launched in October 1957 and was initially used for analgesia, hypnosis and an antiemetic for women in early pregnancy. However, in the following years, the drug caused hundreds of thousands of deformed children in Europe and North America. , so the drug is banned in many countries. However, in recent years, it has been found that the drug has good activity in anti-cancer, immunosuppression, anti-HIV, etc., so it has aroused people's attention again. In 1998, the FDA approved thalidomide for the treatment of concomitant leprosy. Now, in my country, thalidomide is the national essential drug for the treatment of leprosy concomitant diseases. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/04
Inventor 殷学治郭乙杰王兵计莹
Owner CHANGZHOU PHARMA FACTORY
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