HRID1590103

反应详情

EQUATION

反应方程式

HRID 1590103 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 22.7 g 1-(4-methoxyphenyl)hydrazine hydrochloride and 24.6 g methyl 5-t-butylthio-2,2-dimethyl-4-oxopentanoate in 500 mL of t-BuOH was heated at reflux under nitrogen for 24 hours. The solvent was removed under reduced pressure and the residue stirred in 900 mL ether. Filtration and evaporation of the Et2O provided an oil which was chromatographed (silica gel; 3% EtOAc in toluene) to provide the title compound as an oil.

WORKUP

后处理

  1. temperatureat reflux under nitrogen for 24 hours
  2. customThe solvent was removed under reduced pressure
  3. filtrationFiltration and evaporation of the Et2O
  4. customprovided an oil which
  5. customwas chromatographed (silica gel; 3% EtOAc in toluene)