HRID838949

反应详情

EQUATION

反应方程式

HRID 838949 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 6.37 g of the product of Step A, 6.17 g of 4-[3-trifluoromethylphenyl]-1-piperazine-ethanol and 50 ml of anhydrous toluene was refluxed for an hour while passing the condensed toluene through a column filled with siliporite and after cooling to 60° C, 150 mg of sodium hydride were added thereto. The mixture was refluxed with stirring for 16 hours and the toluene was distilled. The product was extracted with methylene chloride, washed with water and dried to obtain 11.6 g of 2-[4-(3-trifluoromethylphenyl)-1-piperazinyl]-ethyl 3-(8-chloro-4-quinolylamino)-2-thiophene-carboxylate.

WORKUP

后处理

  1. temperaturewas refluxed for an hour
  2. additionfilled with siliporite and
  3. temperatureThe mixture was refluxed
  4. distillationthe toluene was distilled
  5. extractionThe product was extracted with methylene chloride
  6. washwashed with water
  7. customdried