HRID2258473
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
6-Amino-3-methyl-1-phenyluracil as obtained in Reference Example 1 (8.7 g, 40 mM) was dissolved in 80 ml of acetic acid and hydrochloric acid (16 ml) was added, followed by heating at 100° C. for 1 hour. The solvent acetic acid was then distilled off under reduced pressure and water war added to the residue. The pH of the resulting solution was adjusted to 1 by adding hydrochloric acid and a product was extracted with dichloromethane. After the solvent dichloromethane was distilled off under reduced pressure from the dichloromethane layer, crystallization with ethanol was performed to give 6-hydroxy-3-methyl-1-phenyluracil (yield: 5.9 g, or 68% based on 6-amino-3-methyl-1-phenyluracil).
WORKUP
后处理
- distillationThe solvent acetic acid was then distilled off under reduced pressure and water war
- additionadded to the residue
- additionby adding hydrochloric acid
- extractiona product was extracted with dichloromethane
- distillationAfter the solvent dichloromethane was distilled off under reduced pressure from the dichloromethane layer, crystallization with ethanol