HRID838947

反应详情

EQUATION

反应方程式

HRID 838947 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 7 g of methyl 3-(8-trifluoromethyl-4-quinolylamino)-2-thiophene-carboxylate, 6.17 g of 4-(3-trifluoromethylphenyl)-1-piperazine-ethanol and 50 ml of anhydrous toluene was refluxed for an hour while passing condensed toluene through a column filled with siliporite and the mixture was cooled to 60° C. 150 mg of sodium hydride were added and the mixture was refluxed with stirring for 10 hours. The toluene was distilled and the residue was extracted with ether, washed with water and dried. The product was crystallized from methylene chloride to obtain 10.9 g of 2-[4-(3-trifluoromethylphenyl)-1-piperazinyl]-ethyl 3-(8-trifluoromethyl-4-quinolylamino)-2-thiophene-carboxylate.

WORKUP

后处理

  1. temperaturewas refluxed for an hour
  2. additionfilled with siliporite and the mixture
  3. temperaturethe mixture was refluxed
  4. distillationThe toluene was distilled
  5. extractionthe residue was extracted with ether
  6. washwashed with water
  7. customdried
  8. customThe product was crystallized from methylene chloride