HRID1160152

反应详情

EQUATION

反应方程式

HRID 1160152 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

A mixture of 3-phenyl-3-hydroxypropylmethanesulfonate (1.71 g, Gao, et al., J. Org. Chem., 1988, 53, 4081), tetrahydrofuran (10 mL) and 28% ammonium hydroxide (30 mL) was heated in a bomb at 65° C. for 16 hours. After cooling, the volatiles were eliminated to leave the aqueous solution which was extracted with ether. The aqueous layer was concentrated under reduced pressure, azeotroped twice with anhydrous acetonitrile and dried under vacuum to give 3-amino-1-phenyl-1-propanol (1.04 g) as a white solid: mp 92-94° C., Rf=0.1 (silica, methanol/ethyl acetate 1/1).

WORKUP

后处理

  1. temperatureAfter cooling
  2. customto leave the aqueous solution which
  3. extractionwas extracted with ether
  4. concentrationThe aqueous layer was concentrated under reduced pressure
  5. customazeotroped twice with anhydrous acetonitrile
  6. customdried under vacuum