HRID2187126

反应详情

EQUATION

反应方程式

HRID 2187126 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 2,2-dimethyl-propionic acid 5-cyano-2-[1-(4fluoro-phenyl)-1-hydroxy-methyl]-benzyl ester (8.0 g, 0.025 mol) in ethylacetate (20 mL) was added hydrogen peroxide solution 30% wt (10 g, 0.079 mol), Na2WO4.2H2O (0.15 g, 0.0005 mol), and (n-Octyl)3NCH3.HSO4 (0.23 g, 0.0005 mol). The mixture was then heated at reflux for 4 hrs, allowed to cool to room temperature and pored into dilute HCl, extracted with diethyl ether (2×50 mL), dried (MgSO4) and concentrated under reduced pressure to give the title ketone compound (7.8 g, 97.5%).

WORKUP

后处理

  1. temperatureThe mixture was then heated
  2. temperatureat reflux for 4 hrs
  3. extractionextracted with diethyl ether (2×50 mL)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated under reduced pressure