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Process for synthesizing chlorquinaldol

A chloroquinaldol and process technology, applied in the field of drug synthesis, can solve problems such as environmental pollution, increase equipment investment, side reactions, etc., and achieve the effects of reducing production cost, less equipment investment, and convenient post-processing

Active Publication Date: 2018-07-31
BEIJING JINCHENG TAIER PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the reaction process using chlorine as the chlorinated raw material, there are a large number of side reactions; and the chlorine used in the synthesis is likely to cause environmental pollution, which increases the investment of a large amount of equipment

Method used

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  • Process for synthesizing chlorquinaldol
  • Process for synthesizing chlorquinaldol

Examples

Experimental program
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Effect test

Embodiment 1

[0019] In a 1000 ml three-necked flask, put 400 grams of 20wt.% hydrochloric acid and 20 grams of 8-hydroxy-2-methylquinoline, cool down to 5°C, add 187 grams of 10wt.% sodium hypochlorite solution dropwise, and control the dropping time 3 hours, during the dropwise addition, control the reaction temperature at 0-10°C, after the dropwise addition, keep it warm for 0.5 hours, and filter to obtain the wet product;

[0020] Put the wet product into 200 ml of purified water, adjust the pH value to 4-5 with sodium carbonate, filter with suction, rinse, and dry to obtain the crude product, which is refined with 200 ml of methanol and 200 ml of purified water to obtain 27.6 g of chloroquinaldol. Yield 96.5%, HPLC purity 99.93%.

Embodiment 2

[0022] In a 1000 ml there-necked flask, put 600 grams of 15wt.% hydrochloric acid and 20 grams of 8-hydroxy-2-methylquinoline, cool down to 15°C, add 187 grams of 10wt.% sodium hypochlorite solution dropwise, and control the dropping time 4 hours, during the dropwise addition, control the reaction temperature at 10-20°C, after the dropwise addition, keep it warm for 0.5 hours, and filter to obtain the wet product;

[0023] Put the wet product into 200 ml of purified water, adjust the pH value to 4-5 with sodium carbonate, suction filter, rinse, and dry to obtain the crude product, which is refined with 200 ml of methanol and 100 ml of purified water to obtain 26.6 g of chloroquinaldol. Yield 92.7%, HPLC purity 99.95%.

Embodiment 3

[0025] In a 1000 ml three-necked flask, put 300 grams of 30wt.% hydrochloric acid and 20 grams of 8-hydroxyl-2-methylquinoline, cool down to 5°C, add 196 grams of 10wt.% sodium hypochlorite solution dropwise, and control the dropping time 5 hours, during the dropwise addition, the reaction temperature was controlled at 0-10°C. After the dropwise addition was completed, keep the temperature for 0.5 hours, and filter to obtain the wet product;

[0026] Put the wet product into 200 ml of purified water, adjust the pH value to 4-5 with sodium carbonate, suction filter, rinse, and dry to obtain the crude product, which is refined with 200 ml of methanol and 300 ml of purified water to obtain 27.2 g of chloroquinaldol. Yield 95.3%, HPLC purity 99.89%.

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Abstract

The invention belongs to the technical field of medicine synthesis, and particularly relates to a process for synthesizing chlorquinaldol. The process comprises the following steps: carrying out reaction between 8-hydroxyl-2-methylquinoline as a raw material and sodium hypochlorite and hydrochloric acid to generate active chlorine atoms as a chlorinated material; performing one-step chlorinated reaction to generate the chlorquinaldol. According to the process disclosed by the invention, using chlorine as a chlorinated material is avoided, and chlorquinaldol is quantitatively generated, so thatthe selectivity and the yield of chlorinated reaction are improved, and meanwhile, the phenomena that pollution on the environment by adopting the chloride and side reaction caused by performing thechlorinated reaction adopting the chloride as the chlorinated material are avoided, and the quality of the chlorquinaldol is ensured.

Description

technical field [0001] The invention belongs to the technical field of medicine synthesis, and in particular relates to a process for synthesizing chloroquinaldol. Background technique [0002] Chloroquinaldol is a yellow needle-like crystal with a slightly pungent odor. It has antimicrobial pathogen activity against fungi, trichomonas, bacteria (G+ and G-), chlamydia and mycoplasma, and is a broad-spectrum antibacterial agent. Developed and manufactured by Theramex Pharmaceutical Factory in Monaco, the disclosed synthesis method is to synthesize 8-hydroxy-2-methylquinoline through a one-step chlorination reaction under the condition of flowing chlorine gas. However, in the reaction process using chlorine gas as the chlorinated raw material, there are a large number of side reactions; and the chlorine gas used in the synthesis is likely to cause environmental pollution, which increases the investment of a large number of equipment. "Chinese Journal of Medicine" published "S...

Claims

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Application Information

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IPC IPC(8): C07D215/28
CPCC07D215/28
Inventor 孙滨张治中王萌张彤李建凯游亚新
Owner BEIJING JINCHENG TAIER PHARMA CO LTD
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