HRID2204163

反应详情

EQUATION

反应方程式

HRID 2204163 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl 4-hydroxy-3-methoxy-benzoate (2.0 g, 11 mmol) in acetone (330 mL) was added K2CO3 (6.1 g, 44 mmol) followed by 1,2-dibromoethane (6.2 g, 2.8 mL, 33 mmol). The mixture was stirred for 2d at 75° C. The mixture was cooled to ambient temperature and the solids were removed by filtration. The filtrate was concentrated and the residue was purified by column chromatography (10-25% ethyl acetate/hexanes) to give methyl 4-(2-bromoethoxy)-3-methoxybenzoate. ESI-MS m/z calc. 288.0, found 289.1 (M+1)+; Retention time: 1.47 minutes (3 min run).

WORKUP

后处理

  1. customthe solids were removed by filtration
  2. concentrationThe filtrate was concentrated
  3. customthe residue was purified by column chromatography (10-25% ethyl acetate/hexanes)