HRID1914622

反应详情

EQUATION

反应方程式

HRID 1914622 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 0.100 g (0.24 mmol) of 4-oxo-2-pyrimidin-4-yl-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidine-9-carboxylic acid N-(4-chloro-2-methoxy-phenyl)-amide (example 1) in 1.00 mL of dimethylformamide was added 0.010 g (0.24 mmol) of sodium hydride at 0° C. and the resulting mixture was stirred at room temperature for 2 hours. 0.020 mL (0.24 mmol) of methyl iodide was added and the mixture was stirred at room temperature for 1 hour. The mixture was dissolved in water and dichloromethane. 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 (cyclohexane/ethyl acetate in proportions of 80/20 to 70/30) to afford 0.053 g (51%) of a solid.

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature for 1 hour
  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 (cyclohexane/ethyl acetate in proportions of 80/20 to 70/30)