HRID1356459

反应详情

EQUATION

反应方程式

HRID 1356459 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
30 °C

PROCEDURE

实验过程

A solution of 4-biphenylmethanol (800 g) in DMF (2.4 l) as cooled to 0° C and thionyl chloride (380 ml) was added to the solution for 40 min. The temperature of the reaction mixture was raised to 30±2° C. and stirring was continued for additional one hr. Methyl 4-hydroxyphenylacetate (722 g) was added and stirring was continued for 20 min at this temperature. 28% Sodium methoxide (2.93 kg) was added to the solution for 70 min and stirring was continued for 6 hr while the temperature of the reaction mixture was maintained at 50±2° C. Water (3.21) was added to the reaction mixture for 25 min while the temperature of the reaction mixture was maintained at 50±2° C. which was stirred for additional one hr at same temperature and cooled to room temperature. The precipitate was collected by filtration and washed with methanol (1.6 l) and water (6.41) sequentially to obtain the titled compound (1119 g).

WORKUP

后处理

  1. stirringstirring
  2. waitwas continued for 20 min at this temperature
  3. stirringstirring
  4. waitwas continued for 6 hr while the temperature of the reaction mixture
  5. temperaturewas maintained at 50±2° C
  6. temperaturewas maintained at 50±2° C. which
  7. stirringwas stirred for additional one hr at same temperature
  8. temperaturecooled to room temperature
  9. filtrationThe precipitate was collected by filtration
  10. washwashed with methanol (1.6 l) and water (6.41) sequentially