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US 2014/0179927 A1Published application
Method for preparation of iloperidone and crystallization method thereof
AssigneeZhejiang Huahai Pharmaceutical Co., Ltd.
InventorsShiwei Zhou, Feng Jian
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Abstract
A method for preparation of iloperidone is provided which comprises reacting 6-fluoro-3-(4-piperidinyl)-1,2-benzoisoxazole hydrochloride with 1-[4-(3-chloropropoxyl)-3-methoxyphenyl]ethyl ketone in an inorganic alkaline aqueous solution. A crystallization method of iloperidone is also provided which comprises adding seed crystal to the iloperidone solution in ethyl acetate, and then iloperidone crystal is obtained with high purity by controlling the temperature and the stirring speed.
Claims8
A crystallization method of iloperidone, characterized in that it comprises the following steps:
- a) crude iloperidone is dissolved under stirring at 70° C.˜80° C. in an appropriate amount of ethyl acetate as a crystallization solvent and then filtered while being hot to remove insoluble impurities in the solution to obtain a clear iloperidone solution;
- b) the resulting iloperidone solution is slowly cooled to 40° C.˜60° C.;
- c) 1% to 5% of iloperidone crystal seed relative to the weight of the crude iloperidone is slowly added thereto;
- d) stirring speed is controlled at 60 r/min-120 r/min, and stirring is performed for 1 hour to 3 hours at a constant temperature;
- e) the resulting solution is slowly cooled to room temperature under stirring, and then continuously stirred for 3 hours to 7 hours;
- f) the resulting crystalline slurry is filtered, and the resulting crystal is washed with ethyl acetate and dried to obtain iloperidone crystal.
3 more elements
Dependencies are inferred from the claim text.