反应详情

温度

30 °C

Pantoprazole free base (50 grams) was dissolved in a solution of tetrahydrofuran (350 ml) and aqueous sodium hydroxide solution (5.4 grams dissolved in 10 ml of water), and stirred at a temperature of 25-35° C. till the clear solution results. The reaction solution was filtered through hyflow and washed the bed with tetrahydrofuran (2×25 ml). Dichloromethane (400 ml) was added slowly to the filtrate over a period of about 1 hour and stirred for about 5-6 hours to crystallize the solid mass. The separated solid mass was cooled to a temperature of 5-10° C. and further stirred for about 2-3 hours. The solid was filtered, washed with dichloromethane (2×25 ml) and suck dried under vacuum. The wet solid was suspended in dichloromethane (250 ml) and stirred for about 15-30 minutes. Then the solid was filtered and suck dried under vacuum and further dried at a temperature of 40-50° C. to afford crystalline Form-I of Pantoprazole sodium sesquihydrate.

1. customresults
2. filtrationThe reaction solution was filtered through hyflow
3. washwashed the bed with tetrahydrofuran (2×25 ml)
4. additionDichloromethane (400 ml) was added slowly to the filtrate over a period of about 1 hour
5. stirringstirred for about 5-6 hours
6. customto crystallize the solid mass
7. temperatureThe separated solid mass was cooled to a temperature of 5-10° C.
8. stirringfurther stirred for about 2-3 hours
9. filtrationThe solid was filtered
10. washwashed with dichloromethane (2×25 ml)
11. customsuck dried under vacuum
12. stirringstirred for about 15-30 minutes
13. filtrationThen the solid was filtered
14. customsuck dried under vacuum
15. customfurther dried at a temperature of 40-50° C.