HRID1788753

反应详情

EQUATION

反应方程式

HRID 1788753 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1,4-dihydro-2-methoxy-6-methyl-4-(3-nitrophenyl)-5-pyrimidinecarboxylic acid, 1-methyethyl ester (2.0 g, 6.0 mmol) in dimethylformamide (7.0 ml) was treated with finely ground potassium carbonate (1.7 g, 12.0 mmoles), N-benzyl-3-chloro-N-methylpropylamine (2.37 g, 12.0 mmol) and a catalytic amount of 18-crown-6. The reaction was heated at 70°-75° C. under argon overnight. The reaction was allowed to cool down to room temperature and was diluted with ether. It was filtered, and the filtrate was washed with water, brine and was dried over anhydrous magnesium sulfate. Evaporation of solvent provided a brown oil which was purified by flash chromatography (20% acetone in hexanes) to yield the title compound (1.51 g) as a yellow oil.

WORKUP

后处理

  1. temperatureThe reaction was heated at 70°-75° C. under argon overnight
  2. filtrationIt was filtered
  3. washthe filtrate was washed with water, brine
  4. dry with materialwas dried over anhydrous magnesium sulfate
  5. customEvaporation of solvent
  6. customprovided a brown oil which
  7. customwas purified by flash chromatography (20% acetone in hexanes)