HRID1701339

反应详情

EQUATION

反应方程式

HRID 1701339 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

1.75 g. of N-acetyl-2-indanamine (0.01 mole) was added to 20 g. of chlorosulfonic acid (0.18 mole), stirred at -60° C. and allowed to warm to 25° C. The mixture was stirred until the reaction was complete, poured into cold water and extracted with ethyl acetate. Evaporation gave the crude N-acetyl-5-chlorosulfonyl-2-indanamine which was converted to N-acetyl-5-sulfamyl-2-indanamine with ammonia in THF. The N-acetyl sulfonamide was purified by recrystallization from water, m.p. 237°-239° C. and hydrolyzed in refluxing 10% hydrochloric acid to give 5-sulfamyl-2-indanamine which was recrystallized from methanol-ether, m.p. 261°-264° C.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. customEvaporation
  3. customgave the crude N-acetyl-5-chlorosulfonyl-2-indanamine which
  4. customThe N-acetyl sulfonamide was purified by recrystallization from water, m.p. 237°-239° C.
  5. temperaturehydrolyzed in refluxing 10% hydrochloric acid