HRID1270082

反应详情

EQUATION

反应方程式

HRID 1270082 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-(3′chloro-2′-cyanophenyl)pyrrole (10 g) in diethyl ether solution was added dropwise to a solution of 1M lithium aluminium hydride in ether solution (100 ml) under nitrogen gas. After addition was complete, the reaction mixture was refluxed for 2 h. and then allowed to stir at room temperature overnight (18 h). The mixture was subsequently quenched with water (4 ml), 2N NaOH (8 ml) and water (16 ml). Stirring was continued for a further 1 h after addition. The crystalline salts were filtered and the filtrate dried over anhydrous magnesium sulphate. After filtering, the ether fitrate was evaporated in vacuo to give the title compound (9.4 g) as a colourless oil.

WORKUP

后处理

  1. additionAfter addition
  2. temperaturethe reaction mixture was refluxed for 2 h.
  3. customThe mixture was subsequently quenched with water (4 ml), 2N NaOH (8 ml) and water (16 ml)
  4. stirringStirring
  5. waitwas continued for a further 1 h
  6. additionafter addition
  7. filtrationThe crystalline salts were filtered
  8. dry with materialthe filtrate dried over anhydrous magnesium sulphate
  9. filtrationAfter filtering
  10. customthe ether fitrate was evaporated in vacuo