HRID2073626

反应详情

EQUATION

反应方程式

HRID 2073626 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.34 g of 5-amino-1,2,3-triazole and 1.0 g of isopropyl α-acetyl-2-fluorocinnamate in 10 ml of acetonitrile is refluxed under heating for 4 hours. The solvent is distilled off under reduced pressure and the residue is crystallized from a mixture of diisopropyl ether and dichloromethane. The resulting crystals are recrystallized from a mixture of methanol, diisopropyl ether and hexane to give 0.3 g of 7-(2-fluorophenyl)-6-isopropoxycarbonyl-5-methyl-4,7-dihydro-1,2,3-triazolo[1,5-a]pyrimidine, melting at 137°-139° C., as colorless crystals.

WORKUP

后处理

  1. temperatureis refluxed
  2. temperatureunder heating for 4 hours
  3. distillationThe solvent is distilled off under reduced pressure
  4. customthe residue is crystallized from a mixture of diisopropyl ether and dichloromethane
  5. customThe resulting crystals are recrystallized from a mixture of methanol, diisopropyl ether and hexane