反应详情

温度

22.5 °C

To a flask equipped with magnetic stirrer, thermometer and nitrogen inlet was added 5-(2-(4-(1,2-benzisothiazol-3-yl)-1-piperazinyl)ethyl)-6-chloro-1,3-dihydro-2H-indol-2-one free base (5.0 g) and dichloromethane (100 mL) and the suspension was stirred at 20-25° C. under nitrogen. A 20.5% anhydrous solution of hydrogen chloride in isopropanol (6.45 g) was added and the mixture was stirred for about 2 h. The product was collected by filtration on a Buchner funnel. The filter cake is rinsed with 3×10 mL of dichloromethane at 20-25° C. and transferred to a drying oven and dried in vacuo at 65-70° C. for about 18 h. The crude material was re-slurried at 20-25° C. for 10 minutes with heptanes and the suspension was filtered in vacuo. The filter cake is rinsed with heptanes at 20-25° C. and transferred to a drying oven and dried in vacuo at 65-70° C. for about 12 h. to afford amorphous ziprasidone hydrochloride having the same PXRD diffractogram, IR and DSC as shown in FIGS. 1 to 3.

1. customTo a flask equipped with magnetic stirrer
2. stirringthe mixture was stirred for about 2 h
3. filtrationThe product was collected by filtration on a Buchner funnel
4. washThe filter cake is rinsed with 3×10 mL of dichloromethane at 20-25° C.
5. customtransferred to a drying oven
6. customdried in vacuo at 65-70° C. for about 18 h
7. filtrationthe suspension was filtered in vacuo
8. washThe filter cake is rinsed with heptanes at 20-25° C.
9. customtransferred to a drying oven
10. customdried in vacuo at 65-70° C. for about 12 h.