反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 22.5 °C
PROCEDURE
实验过程
Quetiapine free base (5.0 g) was dissolved in acetone (50 ml) at room temperature. This was followed by addition of 48% aqueous hydrobromic acid (2 ml) at 30 to 35° C. The resulting solution was stirred for 1 hour at 20 to 25° C. Next, acetone was distilled under vacuum at 40 to 45° C. followed by addition of acetone (50 ml) and distilled under vacuum at 40 to 45° C. till complete removal. Next, acetone (50 ml) and diisopropyl ether (50 ml) were added at 40 to 45° C. The resulted mass was refluxed for 30 minutes and cooled at 20 to 25° C. and further stirred for 2.5 hours. The precipitated product was collected by filtration, washed with diisopropyl ether (25 ml) and dried to give the title compound as white powder (3.8 g).
WORKUP
后处理
- distillationNext, acetone was distilled under vacuum at 40 to 45° C.
- additionfollowed by addition of acetone (50 ml)
- distillationdistilled under vacuum at 40 to 45° C. till complete removal
- additionNext, acetone (50 ml) and diisopropyl ether (50 ml) were added at 40 to 45° C
- temperatureThe resulted mass was refluxed for 30 minutes
- temperaturecooled at 20 to 25° C.
- stirringfurther stirred for 2.5 hours
- filtrationThe precipitated product was collected by filtration
- washwashed with diisopropyl ether (25 ml)
- customdried