HRID1789021

反应详情

EQUATION

反应方程式

HRID 1789021 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

(S)-2,2,2-Trichloro-1-phenylethyl 3-oxobutanoate (8.6 g 27.5 mmoles) and 2,3-dichlorobenzaldehyde (4.82 g, 27.5 mmoles) in dry benzene (100 ml) were heated at reflux for 5 hours with hexanoic acid (25 drops) and piperidine (8 drops) in a Dean and Stark apparatus. The solvent was evaporated and the residue dissolved in ethyl acetate (200 ml), washed with saturated sodium bicarbonate, 2% aqueous sodium bisulphite solution and brine, dried (MgSO4) and the solvent removed in vacuo. The sub-title compound was obtained as a yellow oil. HPLC and nmr indicate 2:1 mixture of geometric isomers.

WORKUP

后处理

  1. customThe solvent was evaporated
  2. dissolutionthe residue dissolved in ethyl acetate (200 ml)
  3. washwashed with saturated sodium bicarbonate, 2% aqueous sodium bisulphite solution and brine
  4. dry with materialdried (MgSO4)
  5. customthe solvent removed in vacuo