HRID2187126
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture was then heated
- temperatureat reflux for 4 hrs
- extractionextracted with diethyl ether (2×50 mL)
- dry with materialdried (MgSO4)
- concentrationconcentrated under reduced pressure