HRID2417979
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customfitted for distillation
- temperatureThe stirred mixture was heated
- distillation1.8 L of distillate was collected over 3 hours
- additionThe reaction was diluted with ethanol (500 ml) and benzene (500 ml)
- filtrationfiltered free of the resin
- concentrationconcentrated to dryness in vacuo
- customThe residue was crystallized from ether and from ethyl acetate