HRID1076829

反应详情

EQUATION

反应方程式

HRID 1076829 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Acetylacetone (9.0 g., 0.09 moles) and ethylurea (7.13 g., 0.081 moles) are dissolved in 30 ml. ethanol. The solution is cooled in an ice-water bath while 30 g. of cold concentrated sulfuric acid is added. The resulting yellow solution is stored at room temperature for 10 days and diluted with a large volume of ether. The ether-ethanol mixture is decanted from the thick syrupy residue which is washed with additional fresh ether. The residue is made basic with 2.5 N sodium hydroxide and extracted throughly with methylene chloride. The organic extracts are dried over sodium sulfate, treated with charcoal, filtered, and evaporated under vacuum affording 1-ethyl-4,6-dimethyl-2(1H)-pyrimidinone as a tan solid (7.6 g., 62%).

WORKUP

后处理

  1. temperatureThe solution is cooled in an ice-water bath while 30 g
  2. customThe ether-ethanol mixture is decanted from the thick syrupy residue which
  3. washis washed with additional fresh ether
  4. extractionextracted throughly with methylene chloride
  5. dry with materialThe organic extracts are dried over sodium sulfate
  6. additiontreated with charcoal
  7. filtrationfiltered
  8. customevaporated under vacuum