HRID1349382

反应详情

EQUATION

反应方程式

HRID 1349382 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 130 ml of 7.9 molar aqueous dimethylamine solution, 16 ml of methanol, 20.0 g of 4-benzyloxycyclohexanone, 23.2 g of dimethylamine hydrochloride and 15.3 g of potassium cyanide was stirred for 65 hours at room temperature; extraction was carried out four times using 120 ml of diethyl ether each time, and the combined extracts were concentrated; 100 ml of dichloromethane were added to the residue, the phases were separated, and the organic phases were dried over sodium sulfate, filtered and concentrated. 24.5 g of 4-benzyloxy-1-dimethylaminocyclohexanecarbonitrile were obtained in the form of a yellowish oil which slowly solidified.

WORKUP

后处理

  1. extractionextraction
  2. concentrationthe combined extracts were concentrated
  3. addition100 ml of dichloromethane were added to the residue
  4. customthe phases were separated
  5. dry with materialthe organic phases were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated