HRID619121

反应详情

EQUATION

反应方程式

HRID 619121 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 0.35 g (1.35 mmol) of 6-amino-4-(2-chloroethyl)-2(1H)-quinolone hydrochloride, 0.33 g (1.5 mmol) of 4-(1-piperazinyl)thieno[3,2-c]pyridine and 0.17 g (2 mmol) of sodium bicarbonate in 10 ml of dimethylformamide is heated to 60° C. for 24 hours. After cooling to room temperature, the reaction medium is diluted in 50 ml of water and the crude product is extracted with chloroform. The organic phase is dried over sodium sulpbate and concentrated. The crude product is purified by flash chromatography on silica, eluting first with a methanol/ethyl acetate (6.5:93.5) mixture containing traces of triethylamine and then with a methanol/dichloromethane (6.5:93.5) mixture comprising traces of aqueous ammonia.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. extractionthe crude product is extracted with chloroform
  3. dry with materialThe organic phase is dried over sodium sulpbate
  4. concentrationconcentrated
  5. customThe crude product is purified by flash chromatography on silica
  6. washeluting first with a methanol/ethyl acetate (6.5:93.5) mixture
  7. additioncontaining traces of triethylamine