HRID406726

反应详情

EQUATION

反应方程式

HRID 406726 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
96 °C

PROCEDURE

实验过程

1-chloro-5-methyl-3-phenylhex-5-en-3-ol (1.28 g, 5.7 mmol), (S)-1-(4-bromophenyl)ethanamine (1.37 g, 1.2 equiv), KI (995 mg, 1.05 equiv), K2CO3 (1.57 g, 2 equiv) were mixed with acetonitrile (15 mL) and heated to reflux (oil bath 96° C.) for overnight. After being cooled to rt, the mixture was filtered, concentrated, and purified by chromatography on a 40-g silica gel column, eluted with 0-8% MeOH in CH2Cl2, to afford 1-((S)-1-(4-bromophenyl)ethylamino)-5-methyl-3-phenylhex-5-en-3-ol (1.33 g, 60%).

WORKUP

后处理

  1. temperatureheated
  2. temperatureAfter being cooled to rt
  3. filtrationthe mixture was filtered
  4. concentrationconcentrated
  5. custompurified by chromatography on a 40-g silica gel column
  6. washeluted with 0-8% MeOH in CH2Cl2