HRID403010

反应详情

EQUATION

反应方程式

HRID 403010 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

3,4-Dibenzyloxybenzaldehyde (27) (22.0 mmol) was suspended in 100 mL of anhydrous methanol and cooled to 0° C. under argon. Sodium borohydride (33.0 mmol) was added in portions to the suspension and stirred for 1 h at the same temperature. The resulting solution was then stirred at room temperature overnight. The reaction mixture was evaporated to dryness and the residue was dissolved in ice-water and neutralized with HCl. The solution was then extracted with chloroform and the organic layer was washed successively with water, 10% NaHCO3 solution in water and brine. The organic layer was dried over anhydrous Na2SO4, filtered and evaporated to dryness to provide pure 3,4-Dibenzyloxybenzyl alcohol (28) in 97.5% yield.

WORKUP

后处理

  1. stirringThe resulting solution was then stirred at room temperature overnight
  2. customThe reaction mixture was evaporated to dryness
  3. dissolutionthe residue was dissolved in ice-water and neutralized with HCl
  4. extractionThe solution was then extracted with chloroform
  5. washthe organic layer was washed successively with water, 10% NaHCO3 solution in water and brine
  6. dry with materialThe organic layer was dried over anhydrous Na2SO4
  7. filtrationfiltered
  8. customevaporated to dryness