HRID421566

反应详情

EQUATION

反应方程式

HRID 421566 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. distillationNext, acetone was distilled under vacuum at 40 to 45° C.
  2. additionfollowed by addition of acetone (50 ml)
  3. distillationdistilled under vacuum at 40 to 45° C. till complete removal
  4. additionNext, acetone (50 ml) and diisopropyl ether (50 ml) were added at 40 to 45° C
  5. temperatureThe resulted mass was refluxed for 30 minutes
  6. temperaturecooled at 20 to 25° C.
  7. stirringfurther stirred for 2.5 hours
  8. filtrationThe precipitated product was collected by filtration
  9. washwashed with diisopropyl ether (25 ml)
  10. customdried