HRID2260935

反应详情

EQUATION

反应方程式

HRID 2260935 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-(2,6,6-trimethylcyclohex-3-enyl)but-2-en-1-one (83.0 g, 0.50 mol, 2 equiv.), ethyl diisopropylamine (32.3 g, 0.25 mol, 1 equiv.) and L-Cystein ethyl ester hydrochloride (46.5 g, 0.25 mol, 1 equiv.) in EtOH (600 ml) is heated to 60° C. during 44 h. The solvent is removed in vacuo and the residue dissolved in methyl t-butyl ether. The solution is washed with dilute aq. NaCl, dried over MgSO4 and concentrated. The residue is purified by chromatography on SiO2 to yield 85.5 g (71%) of the title compound as orange oil.

WORKUP

后处理

  1. customThe solvent is removed in vacuo
  2. dissolutionthe residue dissolved in methyl t-butyl ether
  3. washThe solution is washed with dilute aq. NaCl
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. customThe residue is purified by chromatography on SiO2