HRID2258474

反应详情

EQUATION

反应方程式

HRID 2258474 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

To the obtained 6-hydroxy-3-methyl-1-phenyluracil (12.2 g, 56 mM) was added phosphorus oxychloride (phosphoryl chloride, 167 ml, 2M) under cooling with ice and 3.4 ml of water was then added dropwise. The solution was heated gradually and maintained at 110° C. for 2 hours. The solvent was distilled off under reduced pressure. A product was obtained by crystallization with water and recovered by filtration to yield 6-chloro-3-methyl-1-phenyluracil (yield: 9.55 g, or 72% based on 6-hydroxy-3-methyl-1-phenyluracil).

WORKUP

后处理

  1. additionwas then added dropwise
  2. temperatureThe solution was heated gradually
  3. distillationThe solvent was distilled off under reduced pressure
  4. customA product was obtained by crystallization with water
  5. filtrationrecovered by filtration