HRID2248606

反应详情

EQUATION

反应方程式

HRID 2248606 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 5.7 g (50.8 mmol) of 75% pure 1-amino-1H-1,2,4-triazole, 5.0 g (25.5 mmol) of deoxybenzoin and 0.6 g p-toluenesulfonic acid in 150 mL of benzene was heated at reflux with azeotropic removal of water for 7 days. Solvent was stripped and the residue was diluted with ether, which was washed with saturated aqueous Na2CO3, water and brine. Drying (MgSO4) and removal of solvent gave an off-white solid which was recrystallized from hexane affording 3.23 g of the desired product, m.p. 78°-80° C.

WORKUP

后处理

  1. washwas washed with saturated aqueous Na2CO3, water and brine
  2. customDrying
  3. custom(MgSO4) and removal of solvent
  4. customgave an off-white solid which
  5. customwas recrystallized from hexane affording 3.23 g of the desired product, m.p. 78°-80° C.