乙醇 → 1-ethyl-4,6-dimethyl-2(1H)-pyrimidinone

HRID 1076829

反应方程式

HRID 1076829 反应方程式
[C:1]([CH2:4][C:5](=O)[CH3:6])(=O)[CH3:2].[CH2:8]([NH:10][C:11]([NH2:13])=[O:12])[CH3:9].C(O)C.S(=O)(=O)(O)O>CCOCC>[CH2:8]([N:10]1[C:1]([CH3:2])=[CH:4][C:5]([CH3:6])=[N:13][C:11]1=[O:12])[CH3:9]

参与物

6

反应物 4

HCID 702乙醇HCID 1118四氧化硫HCID 12254N-乙基脲HCID 31261乙酰丙酮

产物 1

HCID 17114931-ethyl-4,6-dimethyl-2(1H)-pyrimidinone

试剂、催化剂与溶剂 1

HCID 3283乙醚溶剂

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%).

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

来源与证据

ORD记录
ord-a80bc0d08b8e4c15af9abe6049989d76
来源数据集
uspto-grants-1976_05
专利号
US03957997

关联笔记

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