HRID2417979

反应详情

EQUATION

反应方程式

HRID 2417979 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The methanolic solution of (2S)-3-(4-benzyloxyphenoxy)-1,2-propanediol acetonide (~2 L) from the previous example was diluted with 120 ml water and combined with Dowex 50W-8X ion exchange resin (50 ml) in a flask fitted for distillation. The stirred mixture was heated to boiling and 1.8 L of distillate was collected over 3 hours. The reaction was diluted with ethanol (500 ml) and benzene (500 ml) filtered free of the resin and concentrated to dryness in vacuo. The residue was crystallized from ether and from ethyl acetate to give 137.0 g of (2R)-3-(4-benzyloxyphenoxy)-1,2-propanediol in several crops.

WORKUP

后处理

  1. customfitted for distillation
  2. temperatureThe stirred mixture was heated
  3. distillation1.8 L of distillate was collected over 3 hours
  4. additionThe reaction was diluted with ethanol (500 ml) and benzene (500 ml)
  5. filtrationfiltered free of the resin
  6. concentrationconcentrated to dryness in vacuo
  7. customThe residue was crystallized from ether and from ethyl acetate