HRID31073

反应详情

EQUATION

反应方程式

HRID 31073 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

5,6-Diamino-1-(4-methoxybenzyl)-2-thioxo-2,3-dihydro-1H-pyrimidin-4-one (0.83 g, 3.0 mmol) was dissolved in formic acid (3.0 mL) and the resulting solution heated at 100° C. for 1 h. The excess formic acid was removed under reduced pressure and the residue dissolved in 10% potassium hydroxide solution (8 mL) and heated at 100° C. for 15 minutes. The reaction mixture was neutralized with 10% acetic acid and the resulting precipitate collected by filtration. The precipitate was recrystallised from ethanol: dimethylformamide and the isolated crystals dissolved in 1M potassium hydroxide solution, precipitated by neutralization with 10% acetic acid and collected by filtration. After drying, the title compound (0.14 g, 16%) was obtained.

WORKUP

后处理

  1. customThe excess formic acid was removed under reduced pressure
  2. dissolutionthe residue dissolved in 10% potassium hydroxide solution (8 mL)
  3. temperatureheated at 100° C. for 15 minutes
  4. filtrationthe resulting precipitate collected by filtration
  5. customThe precipitate was recrystallised from ethanol
  6. dissolutiondimethylformamide and the isolated crystals dissolved in 1M potassium hydroxide solution
  7. customprecipitated by neutralization with 10% acetic acid
  8. filtrationcollected by filtration
  9. customAfter drying