HRID1251945

反应详情

EQUATION

反应方程式

HRID 1251945 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

A suspension of 17.9 g of 7-chloro-1,2-benzisothiazole-1,1-dioxide in 180 ml of absolute ethanol was cooled to 0° C. and treated with 3.33 g of sodium borohydride at such a rate that the temperature remained below 5° C. The mixture was warmed to room temperature for 30 minutes, recooled to 0° C. and treated with glacial acetic acid to destroy excess hydride. The mixture was concentrated to dryness, the resulting solid suspended in water, filtered, washed with water and dried in vacuo at 50° C. for 16 hours to give 17.6 g of the title compound as a white powder, m.p. 159°-161° C.

WORKUP

后处理

  1. customremained below 5° C
  2. temperatureThe mixture was warmed to room temperature for 30 minutes
  3. customrecooled to 0° C.
  4. customto destroy excess hydride
  5. concentrationThe mixture was concentrated to dryness
  6. filtrationfiltered
  7. washwashed with water
  8. customdried in vacuo at 50° C. for 16 hours