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目的:改进绿卡色林盐酸盐半水合物晶型的制备方法。方法:将绿卡色林游离碱完全溶于二氯甲烷中,向反应液中通入氯化氢气体至饱和后,减压蒸馏除去溶剂得到绿卡色林盐酸盐,之后将绿卡色林盐酸盐完全溶解于二氯甲烷中,加入水,搅拌,减压蒸馏除去溶剂,得到油状物,向油状物中加入乙酸乙酯,搅拌,得到绿卡色林盐酸盐半水合物晶型。结果与讨论:该方法无需控制氯化氢气体通入量以及无需通过加热实现转晶过程,具有反应条件易于控制、温和、收率高、产品质量好、适于工业化生产等优点。
OBJECTIVE: To improve the preparation method of green Caracrine hydrochloride hemihydrate crystal. Methods: The green cassosine free base was completely dissolved in methylene chloride, hydrogen chloride gas was passed into the reaction liquid to saturation, the solvent was removed under reduced pressure to get the green caraclin hydrochloride, and then the green caraclin hydrochloride was completely Was dissolved in methylene chloride, water was added and the mixture was stirred. The solvent was distilled off under reduced pressure to give an oil. Ethyl acetate was added to the oil and stirred to give the green-kashaline hydrochloride hemihydrate crystal. Results and discussion: The method has the advantages of easy control of reaction conditions, mildness, high yield, good product quality, suitable for industrialized production, etc., without controlling the amount of hydrogen chloride gas introduced and without the need of heating to achieve the crystal conversion process.