A kind of preparation method of risperidone crystal Ⅲ type substance
A technology for risperidone and substances, which is applied in the field of preparation of risperidone crystal type III substances, can solve problems such as harm to production personnel, and achieve the effects of non-toxic solvent and cost saving
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Embodiment 1
[0019] 100g of crude risperidone, 750g of water, 400g of ethanol, 40g of propylene glycol, and 10g of molecular sieve, mixed and stirred, heated to 40°C, kept for 30 minutes, filtered while hot to remove the molecular sieve, and then the obtained filtrate was placed at -30°C for pre-treatment. Freeze for 6 hours, raise the temperature to -20°C for 3 hours, raise the temperature to -5°C for 3 hours, then raise the temperature to 20°C for 4 hours, and finally raise the temperature to 65°C for 3 hours, and set the heating rate to 5°C / min , the purity of the obtained crystal type III risperidone was 99.59%.
Embodiment 2
[0021] 100g of crude risperidone, 700g of water, 350g of ethanol, 45g of propylene glycol, and 8g of diatomaceous earth were mixed and stirred, kept at 5°C for 60 minutes, filtered to remove the diatomite, and then the obtained filtrate was pre-prepared at -40°C. Freeze for 10 hours, raise the temperature to -23°C for 4 hours, raise the temperature to 0°C for 1 hour, then raise the temperature to 30°C for 2 hours, and finally raise the temperature to 80°C for 2 hours, and set the heating rate to 5°C / min. The purity of the obtained crystalline form III risperidone was 99.16%.
Embodiment 3
[0023] 100g of crude risperidone, 800g of water, 450g of ethanol, 35g of propylene glycol, and 20 g of diatomaceous earth were mixed and stirred, kept at 60°C for 10 minutes, filtered to remove the diatomite, and then the obtained filtrate was pre-prepared at -25°C. Freeze for 3 hours, raise the temperature to -15°C for 1 hour, raise the temperature to -10°C for 4 hours, then raise the temperature to 10°C for 6 hours, and finally raise the temperature to 40°C for 4 hours, and set the heating rate to 5°C / min , the purity of the obtained crystal type III risperidone was 99.25%.
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