HRID280299

反应详情

EQUATION

反应方程式

HRID 280299 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-methylphenylacetone (1.56 g) and 2-(3-chlorophenyl)-2-hydroxyethanamine (1.81 g) was refluxed in benzene (70 ml) under Dean & Stark conditions for 4 h. The solvent was removed under reduced pressure, replaced with ethanol (100 ml) and the solution hydrogenated using Pt as catalyst. The filtered solution was evaported and the residual oil chromatographed on Kieselgel 60 (150 g). Elution with 1% methanol-chloroform gave the title compound (1.8 g) as an oil. Crystallisation from hexane gave 1.26 g as a 56:44 mixture of diastereoisomers, mp 76-78.

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. customthe residual oil chromatographed on Kieselgel 60 (150 g)
  3. washElution with 1% methanol-chloroform