HRID1787942

反应详情

EQUATION

反应方程式

HRID 1787942 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

To a solution of methoxymethyl 3-(2-methyl-1,3-dioxolan-2-yl)phenyl ether (8.16 g, 36.4 mmol) in ether (200 mL) was added dropwise tert-butyl lithium (1.7 M solution, 26.8 mL, 1.25 equivalents) at −5 to −10° C. The reaction mixture was stirred 15 min before carbon dioxide gas was bubbled in for 5 min. The reaction mixture was allowed to warm slowly in the cold bath to about 10° C., then it was extracted with water. The aqueous layer was acidified with 5 N HCl and extracted with EtOAc. The organic phase was dried (MgSO4) and evaporated to afford a crude product which was triturated with hexane to afford the benzoic acid (4.54 g).

WORKUP

后处理

  1. customwas bubbled in for 5 min
  2. extractionit was extracted with water
  3. extractionextracted with EtOAc
  4. dry with materialThe organic phase was dried (MgSO4)
  5. customevaporated
  6. customto afford a crude product which
  7. customwas triturated with hexane