HRID589537

反应详情

EQUATION

反应方程式

HRID 589537 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. distillationthe Ethanol was distilled out
  2. customThe reaction was quenched
  3. additionby adding 132 ml of water
  4. temperatureby heating to 50° C.-60° C. for 2 hours
  5. extractionextracted with ethyl acetate
  6. washThe organic layer was washed with water
  7. customevaporated to dryness
  8. customThe precipitate was crystallized from toluene