HRID334982

反应详情

EQUATION

反应方程式

HRID 334982 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

Potassium hydroxide (0.527 Kg, 9.4 mol) was added to a stirred suspension of methyl 2,4-bis-benzyloxy-5-isopropenyl-benzoate (3.1 Kg, 8 mol, step 4) in methanol (18.6 L) and water (12.4 L) and the mixture was stirred and held at reflux for 3 hours. The methanol was removed under partial vacuum from the vessel, and to the remaining solution was added toluene (62 L). The solution was heated to 40° C. and to the mixture was added conc HCl (1.36 L). The biphasic mixture is heated to 50° C. and the phases separated. The organic phase was washed with water (31 L) at 50° C. and the organic phase was evaporated under redeuced pressure to give 2,4-bis-benzyloxy-5-isopropenyl-benzoic acid 2.851 Kg (95% yield) as a colourless solid.

WORKUP

后处理

  1. temperatureat reflux for 3 hours
  2. customThe methanol was removed under partial vacuum from the vessel
  3. additionto the remaining solution was added toluene (62 L)
  4. additionwas added conc HCl (1.36 L)
  5. temperatureThe biphasic mixture is heated to 50° C.
  6. customthe phases separated
  7. washThe organic phase was washed with water (31 L) at 50° C.
  8. customthe organic phase was evaporated under redeuced pressure