HRID30621

反应详情

EQUATION

反应方程式

HRID 30621 的结构方程式

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

A mixture of 4-fluoroaniline (11.1 g), ethyl formate (25.0 g) and ethanol (150 ml) was stirred at 65° C. for 2 hrs. Toluenesulfonylmethyl isocyanide (23.4 g) was added to the reaction mixture and the mixture was stirred for 2 hrs. with heating under reflux. The reaction mixture was concentrated and poured into water. The precipitated solids were collected by filtration, washed with water and dried to give ethyl 1-(4-fluorophenyl)-1H-imidazole-5-carboxylate (19.8 g, 85%). Recrystallization thereof from ethyl acetate-hexane gave pale-yellow prism crystals. melting point: 114-115° C.

WORKUP

后处理

  1. stirringthe mixture was stirred for 2 hrs
  2. temperaturewith heating
  3. temperatureunder reflux
  4. concentrationThe reaction mixture was concentrated
  5. additionpoured into water
  6. filtrationThe precipitated solids were collected by filtration
  7. washwashed with water
  8. customdried