HRID429817

反应详情

EQUATION

反应方程式

HRID 429817 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
22 °C

PROCEDURE

实验过程

A mixture of 1-(4-bromophenyl)propan-2-one (5 grams, 23.5 mmole), ethylamine hydrochloride (19 grams, 0.23 mole) and sodium cyanoborohydride (2.22 grams, 0.035 mole) in methanol (100 ml) was stirred at 22° C. for 16 hours. The mixture was concentrated under reduced pressure and the residue was partitioned between 1.0N sodium hydroxide (25 ml) and ethyl ether (60 ml). The organic phase was dried (anhydrous magnesium sulfate) and concentrated under reduced pressure. The oily base was converted to the hydrochloride salt and recrystallized from ethanol/ethyl ether to give [2-(4-bromophenyl)-1-methylethyl]ethylamine hydrochloride (3.8 grams, 58%), m.p. 175-176° C.

WORKUP

后处理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customthe residue was partitioned between 1.0N sodium hydroxide (25 ml) and ethyl ether (60 ml)
  3. dry with materialThe organic phase was dried (anhydrous magnesium sulfate)
  4. concentrationconcentrated under reduced pressure
  5. customrecrystallized from ethanol/ethyl ether