HRID1576327

反应详情

EQUATION

反应方程式

HRID 1576327 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 3.6 g. of 6-aminoveratronitrile, dissolved in 75 ml. of anhydrous benzene, a solution of phenyl lithium (prepared from 0.35 g. of lithium and 3.9 g. of bromobenzene) in 60 ml. of anhydrous diethyl ether is added under a nitrogen atmosphere. After 45 minutes 4.4 g. of 1-cyano-4-(2-furoyl)piperazine in 50 ml. of anhydrous benzene are added. The ether and part of the benzene are distilled off and 100 ml. of tetrahydrofuran are added. The mixture is refluxed under the nitrogen atmosphere for 20 hours and then decomposed with water. The liquid is distilled off and 75 ml. of water are added to the residue. The mixture is extracted with chloroform and the extract is concentrated by evaporation of the solvent. 1-(4-Amino-6,7-dimethoxy-2-quinazolinyl)4-(2-furoyl)piperazine is obtained. The product after crystallization from a mixture of ethanol and water melts at 258°-260°C.

WORKUP

后处理

  1. distillationThe ether and part of the benzene are distilled off
  2. additionof tetrahydrofuran are added
  3. temperatureThe mixture is refluxed under the nitrogen atmosphere for 20 hours
  4. distillationThe liquid is distilled off
  5. additionof water are added to the residue
  6. extractionThe mixture is extracted with chloroform
  7. concentrationthe extract is concentrated by evaporation of the solvent