HRID1816596

反应详情

EQUATION

反应方程式

HRID 1816596 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 tetrahydrofuran and 100 ml ethanol. 1 g of sodium borohydride was added thereto, followed by stirring overnight at room temperature. After adding 1 N hydrochloric acid thereto, the reaction solution was extracted with ethyl acetate, and the organic layer was washed with water and brine, 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 N,N-dimethylformamide, and 1.8 g of imidazole and 5.9 g of tertiary butyl chlorodiphenyl silane were added, and the mixture was stirred overnight at room temperature. The reaction mixture was diluted with ethyl acetate, and the organic layer was washed with water and brine, dried over anhydrous magnesium sulfate and the solvent was evpoarated, to give 10.72 g of [(5-bromo-2,3-dimethoxybenzyl)oxy](tertiary butyl)diphenylsilane.

WORKUP

后处理

  1. extractionthe reaction solution was extracted with ethyl acetate
  2. washthe organic layer was washed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated