New method for preparation of meptazinol hydrochloride critical impurity
A key technology of meptafol hydrochloride, which is applied in the field of preparation of key impurity compounds of meptafol hydrochloride, can solve the unqualified quality of meptafol hydrochloride, the inability to remove special impurities, and the process of meptafol hydrochloride issues of immaturity
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Embodiment 1
[0022] To a 50 mL three-necked flask, add 6.18 g of reaction raw materials (III), add 28 mL of dichloromethane, add 3.18 g Na CO , then add 4.90 g of bromoethane, start heating to reflux, and monitor the progress of the reaction by thin layer chromatography (TLC). , reacted for 15 hours, the raw material (III) basically disappeared, stopped heating, cooled, suction filtered, washed the reaction solution with water, and concentrated the organic phase by rotary evaporation to obtain a white slightly yellow solid, which was treated with ethyl acetate-petroleum ether mixed solvent to obtain White solid, which was dried in a forced air drying oven at 40°C for 4 hours to constant weight, weighed to be 5.85 g, yield 85%, MS: 276 [M+H]+.
Embodiment 2
[0024] To a 50 mL three-necked flask, add 6.18 g of reaction raw materials (III), add 22 mL of chloroform, add 3.18 g Na CO , then add 4.90 g of bromoethane, start heating to reflux, and monitor the progress of the reaction by thin layer chromatography (TLC). , reacted for 9 hours, the raw material (III) basically disappeared, stopped heating, cooled, suction filtered, washed the reaction solution with water, and concentrated the organic phase by rotary evaporation to obtain a white slightly yellow solid, which was treated with an ethyl acetate-petroleum ether mixed solvent to obtain White solid, which was dried in a forced air drying oven at 40°C for 4 hours to constant weight, weighed to be 6.20 g, yield 90%, MS: 276 [M+H]+.
Embodiment 3
[0026] To a 50 mL three-necked flask, add 6.18 g of reaction raw materials (III), add 22 mL of chloroform, 6.62 g Na CO , chloroethane 3.22 g, 0.25 g KI, start heating to reflux, monitor the reaction by thin layer chromatography (TLC) and carry out Situation, reacted for 20 hours, the raw material (III) basically disappeared, stopped heating, cooled, suction filtered, washed the reaction solution with water, concentrated the organic phase by rotary evaporation to obtain a white slightly yellow solid, which was treated with an ethyl acetate-petroleum ether mixed solvent A white solid was obtained, and the solid was dried in a forced air drying oven at 40° C. for 4 hours to a constant weight, and the weight was 4.95 g, yield 72%, MS: 276 [M+H]+.
[0027] Example: Preparation of impurity 3-(3-ethoxyphenyl)-3-ethyl-1-methylhomopiperidine
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