HRID1978847

反应详情

EQUATION

反应方程式

HRID 1978847 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.97 ml of methyl cyanoacetate and 0.3 ml of piperidine were added to a solution of 3.3 g of 3-(4-chloro-3-formylphenyl)-2,4-dioxo-1-methyl-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine in 100 ml of tetrahydrofuran. After the mixture had been stirred for 5 hours at the reflux temperature, a further 0.97 ml of methyl cyanoacetate was added and refluxing was continued for a further 5 hours. The reaction mixture was evaporated down and the oil obtained was chromatographed (dichloromethane). The solid obtained was stirred with diisopropyl ether, isolated, washed with petroleum ether and dried.

WORKUP

后处理

  1. temperaturerefluxing
  2. waitwas continued for a further 5 hours
  3. customThe reaction mixture was evaporated down
  4. customthe oil obtained
  5. customwas chromatographed (dichloromethane)
  6. customThe solid obtained
  7. customisolated
  8. washwashed with petroleum ether
  9. customdried