HRID1198638

反应详情

EQUATION

反应方程式

HRID 1198638 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a suspension of 1.90 g (41 mmole) of NaNH2 in 60 ml of dry toluene, 5.50 g (35 mmole) of 2-cyclopentylidene cyclopentanone was added dropwise below about 30° C. under stirring. The resulting mixture was stirred at about room temperature until no NH3 was evolved and then 3.8 g (32 mmole) of 2-dimethylaminoethyl chloride was added dropwise. The mixture was heated for about 2 hours at about 100° C. under stirring. On cooling, the mixture was acidified with 2N HCl. The aqueous layer was separated and the organic layer was extracted with 2N HCl. The combined aqueous layer was basified with 10% NaOH and extracted with ether. The ether extracts were dried over anhydrous MgSO4. The ether solution was treated with ethanolic hydrogen chloride to give 2-(1-cyclopenten-1-yl)-2-dimethylamino-ethyl cyclopentanone hydrochloride.

WORKUP

后处理

  1. additionwas added dropwise below about 30° C.
  2. stirringunder stirring
  3. temperatureOn cooling
  4. customThe aqueous layer was separated
  5. extractionthe organic layer was extracted with 2N HCl
  6. extractionextracted with ether
  7. dry with materialThe ether extracts were dried over anhydrous MgSO4
  8. additionThe ether solution was treated with ethanolic hydrogen chloride