Synthetic technology of chlorquinaldol

A technology of chloroquinadol and synthesis process, applied in the field of drug synthesis, can solve the problems of large amount of sodium hypochlorite solution, increased cost of treating waste liquid, large water content, etc., and achieves increased conversion rate and yield, reduced operation, and reduced waste. effect of liquid

Active Publication Date: 2019-08-20
BEIJING JINCHENG TAIER PHARMA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] This process reduces the pollution of chlorine gas, but still uses corrosive hydrochloric acid, and the concentration of sodium hypochlorite solution is low, and the water content is large, and the product generated by the reaction will be dissolved during the reaction, resulting in a decrease in yield, and the amount of sodium hypochlorite solution is large, resulting in There is more waste liquid, which increases the cost of waste liquid treatment

Method used

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  • Synthetic technology of chlorquinaldol
  • Synthetic technology of chlorquinaldol
  • Synthetic technology of chlorquinaldol

Examples

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Effect test

Embodiment 1

[0027] A kind of synthetic technique of chloroquinaldol: under the dark condition, in the four-neck bottle of 250 milliliters, drop into 100 grams of dichloromethane and 10 grams of 8-hydroxyl-2-methylquinoline, cool to-5 ℃, add 16.8 g of N-chlorosuccinimide and 0.08 g of aluminum chloride were incubated at 0±5°C for 12 hours, filtered with suction, and the solvent was concentrated to obtain crude chloroquinaldol. Refined with 135 grams of ethanol and 45 grams of purified water to obtain chloroquinaldol with a yield of 98.6% and an HPLC purity of 99.93%.

Embodiment 2

[0029] A kind of synthetic technique of chloroquinaldol: under dark condition, in the four-neck bottle of 500 milliliters, drop into 300 grams of chloroform and 20 grams of 8-hydroxyl-2-methylquinoline, cool to 10 ℃, add 34.42 grams of N - chlorosuccinimide and 0.34 g of aluminum chloride, heat at 15±5° C. for 10 hours, filter with suction, and concentrate the solvent to obtain crude chloroquinaldol. Refined with 266 grams of ethanol and 14 grams of purified water to obtain chloroquinaldol with a yield of 98.2% and an HPLC purity of 99.91%.

Embodiment 3

[0031] A kind of synthetic technique of chloroquinaldol: under dark condition, in the four-neck bottle of 500 milliliters, drop into 200 grams of chloroform and 20 grams of 8-hydroxyl-2-methylquinoline, add 32.75 grams of N-chlorobutane Imide and 0.51 g of aluminum chloride were heated up to 55±5°C and kept for 6 hours, filtered with suction, and the solvent was concentrated to obtain crude chloroquinaldol. Refined with 238 grams of ethanol and 42 grams of purified water to obtain chloroquinaldol with a yield of 98.4% and an HPLC purity of 99.96%.

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Abstract

The invention belongs to the field of pharmaceutical synthesis technology and specifically relates to a synthetic technology of chlorquinaldol. By using Lewis acid as a catalyst, 8-hydroxy-2-methylquinoline and N-Chlorosuccinimide, which are used as raw materials, are subjected to a one-step chlorination reaction to generate chlorquinaldol; and after the reaction, chlorquinaldol is refined to obtain the chlorquinaldol. By using N-Chlorosuccinimide to replace chlorine as the raw material of the chlorination reaction, the selectivity is good, side reaction is reduced, conversion rate and yield are increased, yield reaches 98.2% and above, purity is 99.90% and above, quality of the chlorquinaldol is guaranteed, generation of spend liquor is decreased, environmental pollution is reduced, the cost is saved, water dissolution of the reaction product is avoided, and the yield is increased. The technology of the invention is a green and environmentally-friendly technology, and is suitable forindustrial production.

Description

technical field [0001] The invention belongs to the technical field of drug synthesis, and in particular relates to a synthesis process of 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 produced by Theramex Pharmaceutical Factory in Monaco, the disclosed synthesis method is to synthesize 8-hydroxy-2-methylquinoline as raw material, chlorine gas as chlorinated raw material, and undergo a one-step chlorinated reaction. The reaction equation is as follows: [0003] [0004] The chlorine gas used for the synthesis of this reaction is highly toxic, and hydrochloric acid is corrosive, which can easily cause environmental pollution. There are a lot of side reactions in the reaction process, the conversion rate is low, and there a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/28
CPCC07D215/28
Inventor 王琨张忠政张宾张国斌张治中张彤李宗奇
Owner BEIJING JINCHENG TAIER PHARMA CO LTD
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