HRID35668

反应详情

EQUATION

反应方程式

HRID 35668 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-4-oxo-1-propionyl-1,2,3,4-tetrahydroquinoline (2 g), N,N-dimethylformamide dimethyl acetal (7.009 g), and triethylamine (0.87 g) in benzene (50 m) was refluxed with stirring for 1 hour and then about three-fourths of the solvent was distilled slowly at atmospheric pressure over a period ximately 1 hour. To the residue was added benzene (100 ml) and the solvent was distilled again. The resulting solid was collected by filtration, washed with diethyl ether, and dried to give 6-chloro-3-methylaminomethylene-4-oxo-1-propionyl-1,2,3,4-tetrahydroquinoline (2.02 g).

WORKUP

后处理

  1. distillationabout three-fourths of the solvent was distilled slowly at atmospheric pressure over a period ximately 1 hour
  2. additionTo the residue was added benzene (100 ml)
  3. distillationthe solvent was distilled again
  4. filtrationThe resulting solid was collected by filtration
  5. washwashed with diethyl ether
  6. customdried