HRID1296204

反应详情

EQUATION

反应方程式

HRID 1296204 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

10.67 g of 5-bromo-2,3-dimethoxybenzaldehyde was dissolved in 100 ml of tetrahydrofuran and 100 ml of ethanol, and 1 g of sodium borohydride was added, and then the solution was stirred overnight at room temperature. 1 N hydrochloric acid was added thereto, followed by extracting with ethyl acetate. The organic layer was washed with water and an aqueous saturated sodium chloride, dried over anhydrous magnesium sulfate and the solvent was evaporated, to give 10.27 g of 5-bromo-2,3-dimethoxybenzyl alcohol. 5.326 g of this crude product was dissolved in 50 ml of N,N-dimethylformamide, and 1.8 g of imidazole and 5.9 g of t-butylchlorodiphenylsilane were added thereto, and the solution was stirred overnight at room temperature. The reaction mixture was diluted with ethyl acetate, and the organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate and the solvent was evaporated, to give 10.72 g of [(5-bromo-2,3-dimethoxybenzyl)oxy](t-butyl)diphenylsilane.

WORKUP

后处理

  1. extractionby extracting with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialan aqueous saturated sodium chloride, dried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated