HRID2181646

反应详情

EQUATION

反应方程式

HRID 2181646 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

A stirred mixture of methyl benzofuran-5-carboxylate (1.3 g, 7.38 mmol) in MeOH (51 mL) and sodium hydroxide (41 mL of a 5% aqueous solution) is heated to 65° C. for 4 h. The mixture is cooled to rt, and MeOH is removed in vacuo. The remaining aqueous layer is extracted with CH2Cl2. The CH2Cl2 layer is discarded, and the aqueous layer is acidified to pH=1 with concentrated hydrochloric acid. The aqueous layer is extracted with CHCl3. The organic layer is washed with water, dried (MgSO4), filtered and concentrated in vacuo to afford 1.2 g (98%) of benzofuran-5-carboxylic acid as a white solid. 1H NMR (400 MHz, DMSO-d6) δ 12.9, 8.30, 8.11, 7.92, 7.69, 7.09.

WORKUP

后处理

  1. temperatureThe mixture is cooled to rt
  2. customMeOH is removed in vacuo
  3. extractionThe remaining aqueous layer is extracted with CH2Cl2
  4. extractionThe aqueous layer is extracted with CHCl3
  5. washThe organic layer is washed with water
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo