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Synthetic process of chloroquinaldol
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A technology of chloroquinaldol and process, which is applied in the field of drug synthesis and can solve problems such as increased equipment investment, side reactions, and environmental pollution
Active Publication Date: 2021-04-09
BEIJING JINCHENG TAIER PHARMA CO LTD
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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
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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.% sodiumhypochlorite 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 sodiumcarbonate, 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 drug synthesis, and in particular relates to a process for synthesizing chloroquinaldol. The process uses 8-hydroxy-2-methylquinoline as a raw material, uses a chlorine atom in an active state generated by the reaction of sodiumhypochlorite and hydrochloric acid as a chlorinated raw material, and generates chloroquinaldol through a one-step chlorination reaction. The method avoids using chlorine gas as a chlorination raw material, quantitatively generates chloroquinaldol, improves the selectivity and yield of the chlorination reaction, and at the same time, avoids the environmental pollution caused by chlorine gas and the side effects of using chlorine gas as the chlorination raw material to carry out the chlorination reaction. The reaction ensures the quality of chloroquinado.
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 antimicrobialpathogen 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...
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