HRID1600534

反应详情

EQUATION

反应方程式

HRID 1600534 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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 (0.83 g) in 10.4 ml of CCl4 --CH2Cl2 (1:1) was added triphenylphosphin (1.04 g), then the mixture was refluxed for 40 min. The reaction mixture was ice-cooled and aniline (0.28 g) and triethylamine (0.3 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 (0.58 g).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 40 min
  2. temperaturecooled
  3. customAfter evaporation of the solvent
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. filtrationThe insolubles were filtered off
  6. customthe filtrate was evaporated
  7. customThe residue was purified by chromatography on a silica gel column