HRID400234

反应详情

EQUATION

反应方程式

HRID 400234 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2,2-Dimethoxypropane (12 mL, 97 mmol) was added with stirring to a solution of crude diols A and B, catalytic p-toluenesulfonic acid in acetone (50 mL). The mixture was stirred at room temperature overnight, diluted with ether and washed with aqueous sodium bicarbonate solution (twice). The organic extract was dried (magnesium sulfate), filtered and concentrated. The crude oil was chromatographed on a silica gel column and eluted with 2-10% ethyl acetate in hexanes to obtain dioxane C (5.85 g, 65% overall yield from 4-benzyloxy-2,3-epoxy-1-butanol) as a colorless oil.

WORKUP

后处理

  1. washwashed with aqueous sodium bicarbonate solution (twice)
  2. extractionThe organic extract
  3. dry with materialwas dried (magnesium sulfate)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe crude oil was chromatographed on a silica gel column
  7. washeluted with 2-10% ethyl acetate in hexanes
  8. customto obtain