HRID1356462

反应详情

EQUATION

反应方程式

HRID 1356462 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of methyl 4-(4-biphenylylmethoxy)phenylacetate (2.00 g), N,N-dimethylethylenediamine (1.60 g), 2-hydroxypyridine (573 mg) in methanol (4.0 ml) was heated under reflux under nitrogen for 16 hr and cooled until the temperature of the reaction mixture reached to 60±2° C., to which methanol (8.0 ml) was added. The reaction mixture was heated under reflux for additional one hr and cooled to room temperature. The precipitate was collected by filtration and washed with methanol (4.0 ml to obtain the titled compound (2.18 g).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux under nitrogen for 16 hr
  3. temperaturecooled until the temperature of the reaction mixture
  4. additionwas added
  5. temperatureThe reaction mixture was heated
  6. temperatureunder reflux for additional one hr
  7. filtrationThe precipitate was collected by filtration
  8. washwashed with methanol (4.0 ml