HRID1025522

反应详情

EQUATION

反应方程式

HRID 1025522 的结构方程式

PROCEDURE

实验过程

To a solution of the 2-amino-4-methylthio-6-(4-fluorophenyl)-pyrido(3,2-d)pyrimidine of example 8 (700 mg) in ethanol (20 ml) was added 276 mg sodium. The reaction mixture was refluxed for 5 hours and then cooled down. The solvents were evaporated in vacuo and the crude residue was purified by silica gel flash chromatography, the mobile phase being a mixture of ethanol and dichloromethane, in a volume ratio gradually ranging from 3% to 5% ethanol, thus providing 490 mg of the pure title compound (72% yield), which was characterized by its mass spectrum as follows: MS (m/z): 285 ([M+H]+, 100).

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 5 hours
  2. temperaturecooled down
  3. customThe solvents were evaporated in vacuo
  4. customthe crude residue was purified by silica gel flash chromatography
  5. additiona mixture of ethanol and dichloromethane