| 摘要 |
Anticancer compound FU-0-G pharmaceutical intermediate 2-benzyloxy-5-amino-pyrimidin-4-one synthesis method , comprising the following steps: equiped with a water separator, the reaction vessel was added 130ml cyclohexane solution, 0.62mol benzyl alcohol (3), 0.13 mol solid sodium sulfite, controlling the stirring speed 150-180rpm, elevated temperature to 60-65 C, heated for 3 - 4 h, then the temperature of the solution was reduced to 40--45 C, added 0.71-0.73mol 2,5-diamino-pyrimidin-4-one (2), continued reflux for 5-6 h, cooled and added 300ml sodium chloride solution, divided the aqueous layer, the organic layer was extracted with acetonitrile solution, aqueous layers were combined, low pressure distillation until the solution is clear, the temperature of the solution is reduced to 15 - 20 C, added oxalic acid solution to adjust pH to 1-2, the precipitated solid was filtered, recrystallized from nitromethane solution, got crystalline 2-benzyloxy-5 -amino-pyrimidin-4-one. |
