HRID1095165

反应详情

EQUATION

反应方程式

HRID 1095165 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

To a mixture of 5-bromo-2-hydroxy-benzaldehyde (4 g, 20 mmol), KI (1 g) and K2CO3 (4 g, 29 mmol) in DMF (10 mL) was added 2,2-dimethyl-3-(toluene-4-sulfonyloxy)-propionic acid methyl ester (6.9 g, 24 mmol). The mixture was heated at 140° C. for 2 h, and then cooled to room temperature, partitioned between water and ethyl acetate. The organic layer was washed with water (3×), dried over anhydrous Na2SO4 and concentrated. The residue was purified by column chromatography to give the title compound (5.4 g).

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. custompartitioned between water and ethyl acetate
  3. washThe organic layer was washed with water (3×)
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated
  6. customThe residue was purified by column chromatography