反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- customThe excess formic acid was removed under reduced pressure
- dissolutionthe residue dissolved in 10% potassium hydroxide solution (8 mL)
- temperatureheated at 100° C. for 15 minutes
- filtrationthe resulting precipitate collected by filtration
- customThe precipitate was recrystallised from ethanol
- dissolutiondimethylformamide and the isolated crystals dissolved in 1M potassium hydroxide solution
- customprecipitated by neutralization with 10% acetic acid
- filtrationcollected by filtration
- customAfter drying