HRID1600533
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 suspension of 2-methyl-2-(6-methyl-5-phenyl-2,3-dihydro-4-oxo-4H-1,3-oxazin-3-yl)-propionic acid (1.1 g) in 14 ml of CCl4 --CH2Cl2 (1:1) was added triphenylphosphin (1.38 g), then the mixture was refluxed for 40 min. The reaction mixture was ice-cooled and 3,5-dichlorophenol (0.65 g) and triethylamine (0.4 g) were slowly added, then it was stirred at room temperature for 1 h. After evaporation of the solvent, the residue was dissolved in ethyl acetate. The insolubles were filtered off and the filtrate was evaporated. The residue was purified by chromatography on a silica gel column to get the captioned compound (0.7 g).
WORKUP
后处理
- temperaturethe mixture was refluxed for 40 min
- temperaturecooled
- customAfter evaporation of the solvent
- dissolutionthe residue was dissolved in ethyl acetate
- filtrationThe insolubles were filtered off
- customthe filtrate was evaporated
- customThe residue was purified by chromatography on a silica gel column