HRID278558

反应详情

EQUATION

反应方程式

HRID 278558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of ethyl 4-fluorobenzoate (8.4 g), 1,2,4-triazole (4.14 g) and potassium carbonate (20.7 g) in DMF (30 ml) was stirred at 100° C. for 3 hours and concentrated. To the residue was added dichloromethane, and the mixture was washed with water, dried and concentrated. The residue was purified with silica gel column chromatography (dichloromethane:methanol=50:1→20:1) to give a colorless solid of ethyl 4-(1,2,4-triazol-1-yl)benzoate (4.0 g) and ethyl 4-(1,2,4- triazol-4- yl)benzoate (369 mg).

WORKUP

后处理

  1. concentrationconcentrated
  2. additionTo the residue was added dichloromethane
  3. washthe mixture was washed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was purified with silica gel column chromatography (dichloromethane:methanol=50:1→20:1)