1-(3-吡啶基)-3-(二甲氨基)-2-丙烯-1-酮 → 7-(3-Pyridinyl)[1,2,4]triazolo[1,5-a]pyrimidine

HRID 326089

反应方程式

HRID 326089 反应方程式
[NH2:1][C:2]1[N:6]=[CH:5][NH:4][N:3]=1.CN(C)[CH:9]=[CH:10][C:11]([C:13]1[CH:14]=[N:15][CH:16]=[CH:17][CH:18]=1)=O>C(O)(=O)C>[N:15]1[CH:16]=[CH:17][CH:18]=[C:13]([C:11]2[N:3]3[N:4]=[CH:5][N:6]=[C:2]3[N:1]=[CH:9][CH:10]=2)[CH:14]=1

参与物

4

反应物 2

HCID 5670331-(3-吡啶基)-3-(二甲氨基)-2-丙烯-1-酮HCID 178418311HCID 178418311，化合物

产物 1

HCID 9009447-(3-Pyridinyl)[1,2,4]triazolo[1,5-a]pyrimidine

试剂、催化剂与溶剂 1

HCID 176醋酸溶剂

实验过程

A mixture of 2.54 g of 3-amino-1,2,4-triazole, 5.29 g of 3-dimethylamino-1-(3-pyridyl)-2-propene-1-one and 25 ml of glacial acetic acid was heated under reflux for 6 hours. The solvent was removed in vacuo and the solid residue was partitioned between a saturated aqueous sodium bicarbonate solution and dichloromethane. The organic layer was separated and dried over powdered anhydrous sodium sulfate. This solution was passed through a short column of a hydrous magnesium silicate and the effluent was refluxed on a steam bath with the gradual addition of hexane until crystallization was noted. On cooling the desired compound was separated and collection by filtration gave 1.95 g. of colorless crystals mp. 209°-210° C.

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 6 hours
  3. customThe solvent was removed in vacuo
  4. customthe solid residue was partitioned between a saturated aqueous sodium bicarbonate solution and dichloromethane
  5. customThe organic layer was separated
  6. customdried
  7. temperaturethe effluent was refluxed on a steam bath with the gradual addition of hexane until crystallization
  8. temperatureOn cooling the desired compound
  9. customwas separated
  10. customcollection
  11. filtrationby filtration
  12. customgave 1.95 g

来源与证据

ORD记录
ord-71b0cc88388149b8b5c31ae457814789
来源数据集
uspto-grants-1984_04
专利号
US04444774

关联笔记

加载中…