HRID1356460

反应详情

EQUATION

反应方程式

HRID 1356460 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A suspension of methyl 4-(4-biphenylylmethoxy)phenylacetate (1000 g), N,N-dimethylethylenediamine (795 g), and 1H-1,2,4-triazole (207 g) in methanol (2.0 l) was heated under reflux under nitrogen for 10 hr and was left to stand at room temperature over night. The reaction mixture was warmed to 60±2° C. and methanol (4.0 l) was added for 35 min. After stirring under reflux for additional one hr the reaction mixture was cooled to room temperature. The precipitate was collected by filtration and washed with methanol (2.0 l) to obtain the titled compound (1109 g).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux under nitrogen for 10 hr
  3. waitwas left
  4. waitto stand at room temperature over night
  5. temperatureunder reflux for additional one hr the reaction mixture
  6. temperaturewas cooled to room temperature
  7. filtrationThe precipitate was collected by filtration
  8. washwashed with methanol (2.0 l)