HRID1715686

反应详情

EQUATION

反应方程式

HRID 1715686 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 4-fluorobenzenesulfonyl chloride (3.97 g, 20 mmol) in methylene chloride (40 ml), at 0° C., under nitrogen, with stirring, is added morpholine (4.4 mL, 50 mmol). The mixture is stirred at 0° C. for 15 min. and then warmed to room temperature for 18 hrs. The resulting suspension is filtered, and the filtrate is stirred with 10% potassium carbonate for 2 hrs. The methylene chloride is evaporated, and the aqueous suspension is filtered, and the precipitate is washed with water, and then dried in vacuo to give 5.0 g of a white solid; mp 106-107° C.; MS (APCI) m/z 246.1 (M+H).

WORKUP

后处理

  1. temperaturewarmed to room temperature for 18 hrs
  2. filtrationThe resulting suspension is filtered
  3. stirringthe filtrate is stirred with 10% potassium carbonate for 2 hrs
  4. customThe methylene chloride is evaporated
  5. filtrationthe aqueous suspension is filtered
  6. washthe precipitate is washed with water
  7. customdried in vacuo