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A kind of preparation method of risperidone crystal type I substance

A technology of risperidone and type I, which is applied in the field of preparation of risperidone crystal type I substances, can solve problems such as adverse environmental impact, labor protection difficulties, cumbersome operation, etc., and achieve the effect of reducing the use

Active Publication Date: 2017-10-10
天津市亨必达化学合成物有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has cumbersome operations, it is difficult to obtain a relatively pure single crystal form, a large amount of toxic organic solvents are used, and the solvents are difficult to recover, the cost is high, it brings certain difficulties to labor protection, and has adverse effects on the environment.

Method used

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  • A kind of preparation method of risperidone crystal type I substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Mix 100g of crude risperidone, 800g of water, 500g of ethanol, and 12g of diatomaceous earth, heat to reflux for 1.5 hours at 75°C under stirring, then filter while hot to remove the adsorbent; place the obtained filtrate at 79°C for heating and distillation for 5 hours, the recovered ethanol can be obtained. After the distillation is completed, the solution will be gradually cooled to 25°C, kept for 6 hours, and the cooling rate is set at 5°C / min, filtered, washed, and dried to obtain risperidone crystal type I substance, which can be used The purity of the type I substance of Pertone crystal is 99.62%.

Embodiment 2

[0022] Mix 100 g of crude risperidone, 700 g of water, 400 g of ethanol, and 10 g of molecular sieves, heat to reflux for 2 hours at 60°C under stirring, and then filter while hot to remove the adsorbent; place the obtained filtrate at 75°C and heat and distill for 6 hours. The recovered ethanol can be obtained. After the distillation is completed, the solution will be gradually cooled to 10°C, kept for 4 hours, set the cooling rate at 5°C / min, filtered, washed, and dried to obtain risperidone crystal type I substance, risperidone The purity of the crystalline Form I material was 98.24%.

Embodiment 3

[0024] Mix 100g of crude risperidone, 900g of water, 550g of ethanol, and 20g of activated carbon, heat to reflux at 85°C for 1 hour with stirring, then filter while hot to remove the adsorbent; place the obtained filtrate at 85°C for 4 hours and heat to distill. The recovered ethanol can be obtained. After the distillation is completed, the solution will be gradually cooled to 30°C, kept for 8 hours, set the cooling rate at 5°C / min, filtered, washed, and dried to obtain risperidone crystal type I substance, risperidone The purity of the crystalline Form I material was 98.12%.

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Abstract

The invention provides a preparation method of Risperdal I-type crystal. The preparation method comprises following steps: 1) purification, wherein Risperdal crude product, water, ethanol, and an adsorbent are mixed at a ratio of 1:5-10:3-6:0.005-0.03, an obtained mixture is subjected to 1 to 2h of heating reflux at 60 to 85 DEG C with stirring, and the absorbent is removed via filtering before cooling; and 2) recrystallization, wherein an obtained filtrate is subjected to heating distillation for 3 to 6h at 75 to 85 DEG C so as to obtain recycled ethanol, and white crystal is obtained via precipitation from the filtrate, after distillation, an obtained solution is cooled to 10 to 30 DEG C gradually, and is subjected to thermal insulation for 4 to 8h, and the Risperdal I-type crystal is obtained via filtering, washing, and drying, wherein the cooling speed is controlled to be 5 DEG C / min. The used solvents are nontoxic, and are convenient to recycle, and purity of the obtained Risperdal I-type crystal is as high as 99.62%.

Description

technical field [0001] The invention relates to a preparation method of risperidone crystal type I substance, which belongs to the field of medicine and chemical industry. Background technique [0002] Risperidone belongs to benzisoxazole derivatives in chemical structure, and its chemical name is 3-[2-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1- Piperidinyl]ethyl]-6,7,8,9-tetrahydro-2-methyl-4H-pyrido[1,2-α]pyrimidin-4-one, which has the formula C 23 h 27 FN 4 o 2 , its structural formula is as follows: [0003] [0004] Risperdal was developed by the Belgian Janssen Pharmaceutical Company in 1984, and its trade name is "Risperdal". It is mainly used for the treatment of acute and chronic schizophrenia, especially for positive and negative symptoms and accompanying emotional symptoms (such as anxiety, depression, etc.). It may also reduce affective symptoms associated with schizophrenia. For patients who are effective in the acute phase of treatment, risperidone can con...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D471/04
CPCC07B2200/13C07D471/04
Inventor 张智强王凯李连启刘亚梅马克宋金津李果任晓峰李静雅
Owner 天津市亨必达化学合成物有限公司