HRID2289640

反应详情

EQUATION

反应方程式

HRID 2289640 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-(tert-butyl-dimethyl-silanyloxymethyl)-1-(3-chlorophenyl)-1H-pyridin-2-one (5.11 g, 14.6 mmol) in acetonitrile (75 ml) in a teflon beaker was added hydrogen fluoride-pyridine (2.5 ml, 87.5 mmol) and stirred for 3 hours. The reaction mixture was neutrallized with solid and aqueous sodium dicarbonate and then the solvent evaporated in vacuo. The resulting solid residue was extracted with EtOAc, dried (MgSO4), filtered and the solvent was evaporated in vacuo. This residue was chromatographed (silica gel, 80-100% EtOAc:hexane gradient elution) to afford the title compound.

WORKUP

后处理

  1. customthe solvent evaporated in vacuo
  2. extractionThe resulting solid residue was extracted with EtOAc
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customthe solvent was evaporated in vacuo
  6. customThis residue was chromatographed
  7. wash(silica gel, 80-100% EtOAc:hexane gradient elution)