Synthetic method for macitentan drug intermediate

A synthesis method and technology of macitentan are applied in the field of synthesis of macitentan pharmaceutical intermediates, which can solve the problems of high price and low purity, and achieve the effects of increasing concentration and reducing synthesis cost.

Inactive Publication Date: 2018-12-25
嘉善中嘉化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a kind of synthetic method of macitentan me...

Method used

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  • Synthetic method for macitentan drug intermediate
  • Synthetic method for macitentan drug intermediate
  • Synthetic method for macitentan drug intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Synthesis of monoester: 20 parts of anhydrous methanol, 6 parts of 4-bromophenylacetic acid and 8 parts of sulfonyl chloride are completely mixed in a reactor. After the preliminary mixing, place in the lifting digital control thermostat, set the temperature at 70°C, and slowly turn on the magnetic stirrer. After 4 hours of reaction, the reaction process was terminated. The final product obtained by the reaction was dissolved in ethyl acetate, washed with saturated sodium bicarbonate solution, water, and saturated saline, and finally added with anhydrous sodium sulfate to seal and dry. After drying, the solvent was distilled off under reduced pressure to obtain a colorless transparent oil (monoester).

[0020] (2) Synthesis of diesters from monoesters: After initially mixing 10 parts of monoesters and dimethyl carbonate, the reaction bottle was placed in a lifting numerical control thermostat, and the magnetic stirrer was slowly turned on, and the newly prepared so...

Embodiment 2

[0024] (1) Synthesis of monoester: 25 parts of anhydrous methanol, 7 parts of 4-bromophenylacetic acid and 9 parts of sulfonyl chloride are completely mixed in a reactor. After the preliminary mixing, place in the lifting digital control thermostat, set the temperature at 70°C, and slowly turn on the magnetic stirrer. After 4 hours of reaction, the reaction process was terminated. The final product obtained from the reaction was dissolved in ethyl acetate, washed with saturated sodium bicarbonate solution, water, and saturated saline, and finally added with anhydrous sodium sulfate to seal and dry. After drying, the solvent was distilled off under reduced pressure to obtain a colorless transparent oil (monoester).

[0025] (2) Synthesis of diesters from monoesters: After initially mixing 12 parts of monoesters and dimethyl carbonate, place the reaction bottle in a numerically controlled thermostat. Slowly start the magnetic stirrer, add 30 parts of newly prepared sodium meth...

Embodiment 3

[0029] (1) Synthesis of monoester: 30 parts of anhydrous methanol, 8 parts of 4-bromophenylacetic acid, and 10 parts of sulfonyl chloride are completely mixed in a reactor. After preliminary mixing, place in a lifting digital control thermostat, set the temperature at 70°C, and slowly turn on the magnetic stirrer. After 4 hours of reaction, the reaction process was terminated. The final product obtained by the reaction was dissolved in ethyl acetate, washed with saturated sodium bicarbonate solution, water, and saturated saline, and finally added with anhydrous sodium sulfate to seal and dry. After drying, the solvent was distilled off under reduced pressure to obtain a colorless transparent oil (monoester).

[0030] (2) Synthesis of diesters from monoesters: After initially mixing 15 parts of monoesters and dimethyl carbonate, the reaction bottle was placed in a lifting numerical control thermostat, and the magnetic stirrer was slowly turned on, and newly prepared sodium met...

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Abstract

The invention discloses a synthetic method for a macitentan drug intermediate. The synthetic method for the macitentan drug intermediate comprises the following raw material components: 20-30 parts ofanhydrous methanol, 6-8 parts of 4-bromophenylacetic acid, 8-10 parts of sulfonyl chloride, 20-40 parts of sodium methoxide, 10-15 parts of dimethyl carbonate, 5-10 parts of formamidine hydrochloride, 60-80 parts of phosphorus oxychloride (newly evaporated) and 1-2 parts of N,N-dimethylaniline. According to the provided synthetic scheme, synthetic raw materials are simple, the purity of the obtained product is higher than that of like products, and the requirement for keeping synthesizing macitentan can be met.

Description

technical field [0001] The invention relates to the field of drug synthesis, in particular to a method for synthesizing a macitentan drug intermediate. Background technique [0002] Since the 21st century, the field of biomedicine has developed rapidly, and drug research and its application are very active. At the same time, people's increasing material demand and emphasis on diseases have also accelerated the pace of continuous innovation of new drugs. The efficacy, production cost and safety of new drugs need to be resolved urgently. The abnormal increase of pulmonary artery pressure, the so-called pulmonary arterial hypertension (PAH), has many causes and many of them have not been discovered by the medical field. The disease will eventually lead to right heart failure and even death. The average survival period is only about 3.5 years. The treatment of PAH has always been the focus and difficulty of medical treatment in various countries. The common treatment methods m...

Claims

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Application Information

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IPC IPC(8): C07D239/30
CPCC07D239/30
Inventor 吴学超
Owner 嘉善中嘉化工有限公司
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