HRID653120

反应详情

EQUATION

反应方程式

HRID 653120 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 6-chloro-1-cyclopropyl-carbonyl-4-oxo-1,2,3,4-tetrahydroquinoline (1.996 g), N,N-dimethylformamide dimethyl acetal (3.808 g), and triethylamine (1.212 g) in benzene (16 ml) was refluxed with stirring for 30 minutes and then about three-fourths of the solvent was distilled slowly at atmospheric pressure over a period of approximately 30 minutes. To the residue was added benzene (16 ml) and the solvent was distilled again. The residue was dissolved in ethyl acetate, treated with activated charcoal, and evaporated in vacuo. The residual solid was washed with diethyl ether to give 6-chloro-1-cyclopropyl-carbonyl-3-dimethylaminomethylene-4-oxo-1,2,3,4-tetrahydroquinoline (2.43 g).

WORKUP

后处理

  1. distillationabout three-fourths of the solvent was distilled slowly at atmospheric pressure over a period of approximately 30 minutes
  2. additionTo the residue was added benzene (16 ml)
  3. distillationthe solvent was distilled again
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. additiontreated with activated charcoal
  6. customevaporated in vacuo
  7. washThe residual solid was washed with diethyl ether