HRID2258473

反应详情

EQUATION

反应方程式

HRID 2258473 的结构方程式

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

  1. distillationThe solvent acetic acid was then distilled off under reduced pressure and water war
  2. additionadded to the residue
  3. additionby adding hydrochloric acid
  4. extractiona product was extracted with dichloromethane
  5. distillationAfter the solvent dichloromethane was distilled off under reduced pressure from the dichloromethane layer, crystallization with ethanol