HRID1914621

反应详情

EQUATION

反应方程式

HRID 1914621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a suspension of 0.150 g (0.52 mmol) of (+/−)-4-oxo-2-pyrimidin-4-yl-1,6,7,8-tetrahydro-4H-pyrido[1,2-a]pyrimidine-9-carboxylic acid methyl ester in a sealed tube in 10.00 mL of toluene was added 0.825 g (5.24 mmol) of 4-chloro-2-methoxy-phenylamine and the resulting mixture was stirred under reflux for 16 hours. The mixture was dissolved in water and ethyl acetate. The organic phases were washed with a saturated aqueous solution of sodium chloride, dried over sodium sulfate and evaporated to dryness. The residue was purified by flash chromatography (dichloromethane/methanol/ammoniac in proportions of 100/0/0 to 98/2/02) to afford 0.069 g (32%) of a solid.

WORKUP

后处理

  1. temperatureunder reflux for 16 hours
  2. washThe organic phases were washed with a saturated aqueous solution of sodium chloride
  3. dry with materialdried over sodium sulfate
  4. customevaporated to dryness
  5. customThe residue was purified by flash chromatography (dichloromethane/methanol/ammoniac in proportions of 100/0/0 to 98/2/02)