HRID1755651

反应详情

EQUATION

反应方程式

HRID 1755651 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

20 g (14.03×10-2 mol) of 2,4-dimethyl-6-chloropyrimidine are dissolved in 300 ml of dichloromethane in a 500 ml three-necked flask fitted with a thermometer and a magnetic stirrer. The mixture is cooled to 5° C. and 65.3 g of 55% metachloroperbenzoic acid, which is about 1.5 equivalents, are then added in solid portions. The reaction mixture is then stirred for 24 hours at ambient temperature (25° C.) and then filtered through a 3 frit. The filtrate is washed with 150 ml of a 6% aqueous sodium hydroxide solution and then with 2×50 ml of water to render neutral. It is then dried over sodium sulphate and then filtered through paper and evaporated. The crude mass is recrystallised from n-hexane.

WORKUP

后处理

  1. customfitted with a thermometer and a magnetic stirrer
  2. additionare then added in solid portions
  3. filtrationfiltered through a 3 frit
  4. washThe filtrate is washed with 150 ml of a 6% aqueous sodium hydroxide solution
  5. dry with materialIt is then dried over sodium sulphate
  6. filtrationfiltered through paper
  7. customevaporated
  8. customThe crude mass is recrystallised from n-hexane