HRID893798

反应详情

EQUATION

反应方程式

HRID 893798 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

54.5 g (0.25 mol) of 2-methylsulphonyl-4,6-dimethoxy-pyrimidine, 69 g (0.5 mol) of potassium carbonate and 1500 ml of acetonitrile are mixed with stirring. 33.85 g (0.1375 mol) of O-methyl-isourea sulphate are then added and the mixture is heated to boiling for 17 hours. After cooling, the solution is filtered off with suction and the mother liquor is concentrated. After taking up the residue in methylene chloride, the solution is washed three times with water, dried and concentrated again. 49.9 g of N-(4,6-dimethoxy-pyrimidin-2-yl)-O-methylisourea are obtained in the form of yellow crystals of melting point 91°-95° C. (90% purity; yield 85% of theory).

WORKUP

后处理

  1. temperaturethe mixture is heated
  2. temperatureAfter cooling
  3. filtrationthe solution is filtered off with suction
  4. concentrationthe mother liquor is concentrated
  5. washthe solution is washed three times with water
  6. customdried
  7. concentrationconcentrated again