HRID589537
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
CONDITIONS
反应条件
- 温度
- 6 °C
PROCEDURE
实验过程
Sodium dihydrogen phosphate (58.3 g) was added to a solution of 50 g of diethyl phenylmalonate in 350 ml of ethanol. The mixture was cooled to 5-7° C. and a solution of 16.7 g of sodium borohydride in 38 ml of 0.2% NaOH was gradually added. The mixture was stirred for additional 2 hours and the Ethanol was distilled out. The reaction was quenched by adding 132 ml of water followed by heating to 50° C.-60° C. for 2 hours. The solution was then basified with 50% NaOH and extracted with ethyl acetate. The organic layer was washed with water and evaporated to dryness. The precipitate was crystallized from toluene. 20 g of 2-phenyl-1,3-propanediol was obtained with a yield of 63%.
WORKUP
后处理
- distillationthe Ethanol was distilled out
- customThe reaction was quenched
- additionby adding 132 ml of water
- temperatureby heating to 50° C.-60° C. for 2 hours
- extractionextracted with ethyl acetate
- washThe organic layer was washed with water
- customevaporated to dryness
- customThe precipitate was crystallized from toluene