HRID1058523

反应详情

EQUATION

反应方程式

HRID 1058523 的结构方程式

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Sertraline hydrochloride (125 g) was slurried in a mixture of water (1 L) and (2.5 L). NaOH (25% aqueous, 35 mL) was added. Sertraline base partitioned into the hexane phase. The hexane layer was separated. The aqueous layer was extracted a second time with hexane (500 mL). The hexane layers were combined. The solution of sertraline base in hexane was heated to 50° C. Glacial acetic acid (23 ml) was added to the solution of sertraline base. The reaction mixture was stirred at 50° C. for 30minutes. The reaction mixture was allowed to cool to room temperature and stirred at room temperature overnight. The crystals were filtered and washed five times with a total of 250 mL of hexane. The solids were dried at 40° C. in a vacuum oven for 48 hours. The yield was 89%. mp 126° C.

WORKUP

后处理

  1. customSertraline base partitioned into the hexane phase
  2. customThe hexane layer was separated
  3. extractionThe aqueous layer was extracted a second time with hexane (500 mL)
  4. additionGlacial acetic acid (23 ml) was added to the solution of sertraline base
  5. temperatureto cool to room temperature
  6. stirringstirred at room temperature overnight
  7. filtrationThe crystals were filtered
  8. washwashed five times with a total of 250 mL of hexane
  9. customThe solids were dried at 40° C. in a vacuum oven for 48 hours