HRID1177191

反应详情

EQUATION

反应方程式

HRID 1177191 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of 3,5-bis-benzyloxy-4-bromo-benzoic acid benzyl ester (200a) (225 g, 0.45 mol) in THF (400 mL) and H2O (500 mL) was added NaOH (89.4 g, 2.24 mol) in one portion. The mixture was refluxed for 4 hr. TLC (EtOAc/petroleum ether=1/4) showed that the reaction was complete. Et2O (100 mL) was added to the mixture and the organic layer was separated. The aqueous layer was acidified with conc. HCl, and the resulting solid was filtered and dried in vacuo to give the title compound (150 g, 85% yield) as a white solid. 1H NMR (400 MHz, CDCl3): δ 7.48 (dd, 4 H), 7.39 (t, 4 H), 7.31 (m, 4 H), 5.27 (s, 4 H).

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 4 hr
  2. customthe organic layer was separated
  3. filtrationthe resulting solid was filtered
  4. customdried in vacuo