HRID1058634

反应详情

EQUATION

反应方程式

HRID 1058634 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 0.50 g of 4-chloro-1-[2-(4-piperidyl)ethyl]-1H-imidazo-[4,5-c]quinoline trifluoroacetate and 0.32 g of potassium carbonate in 2 ml of N,N-dimethylformamide, a solution of 0.23 g of p-fluorobenzenesulfonyl chloride in 3 ml of N,N-dimethylformamide was added dropwise at room temperature, and the mixture was stirred for 5 hours. The reaction mixture was adjusted to pH 10 with 10% aqueous sodium hydroxide solution, and extracted with ethyl acetate. The extract was washed successively with water and saturated brine, and dried, and then the solvent was evaporated to give 0.35 g of a colorless solid. Recrystallization from a mixture of methanol, ethanol and water gave colorless crystals having the melting point of from 175 to 178.5° C.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed successively with water and saturated brine
  3. customdried
  4. customthe solvent was evaporated