HRID1179063

反应详情

EQUATION

反应方程式

HRID 1179063 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dimethyl-(8-thiophen-2-yl-1,4-dioxa-spiro[4.5]dec-8-yl)-amine hydrochloride (8.68 g) was dissolved in 7.5M hydrochloric acid (29 ml), stirred for 48 hours at room temperature and then extracted with diethyl ether (2×50 ml). The aqueous phase was rendered alkaline with 5M sodium hydroxide solution, while cooling with ice, extracted with dichloromethane (3×50 ml), dried and concentrated. 4-Dimethylamino-4-thiophen-2-yl-cyclohexanone was obtained as a yellow solid (5.66 g; m.p. 108-110° C.).

WORKUP

后处理

  1. extractionextracted with diethyl ether (2×50 ml)
  2. temperaturewhile cooling with ice
  3. extractionextracted with dichloromethane (3×50 ml)
  4. customdried
  5. concentrationconcentrated