HRID440219

反应详情

EQUATION

反应方程式

HRID 440219 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 250 ml of methanol was dissolved 13.1 g of metal sodium. To the resulting methanol solution were added 25 g (0.28 mol) of N-methylthiourea and 38.5 g (0.29 mol) of dimethyl malonate, and the mixture was reacted under reflux for 3 hours. Thereafter, to the solution was added dropwise 41.3 g (0.29 mol) of methyl iodide at 10° C. or lower, and the mixture was reacted at room temperature overnight. After completion of the reaction, methanol was removed under reduced pressure, and then the residue was dissolved in water. The resulting aqueous solution was made acidic with hydrochloric acid, and crystals precipitated were filtered, washed with water and dried to obtain 42.4 g (yield: 89%) of 6-hydroxy-3-methyl-2-methylthio-4(3H)-pyrimidinone.

WORKUP

后处理

  1. customthe mixture was reacted
  2. temperatureunder reflux for 3 hours
  3. customlower, and the mixture was reacted at room temperature overnight
  4. customwas removed under reduced pressure
  5. dissolutionthe residue was dissolved in water
  6. customprecipitated
  7. filtrationwere filtered
  8. washwashed with water
  9. customdried