5-氨基尿嘧啶 → 6-甲基吡啶并[3,2-D]嘧啶-2,4(1H,3H)-二酮

HRID 1597828笔记

反应方程式

HRID 1597828 反应方程式
[NH2:1][C:2]1[C:3](=[O:9])[NH:4][C:5](=[O:8])[NH:6][CH:7]=1.[CH:10](=O)/[CH:11]=[CH:12]/[CH3:13]>Cl>[O:8]=[C:5]1[NH:6][C:7]2[CH:10]=[CH:11][C:12]([CH3:13])=[N:1][C:2]=2[C:3](=[O:9])[NH:4]1

参与物

4

反应物 2

HCID 136115-氨基尿嘧啶HCID 447466巴豆醛/反丁烯醛

产物 1

HCID 2732406-甲基吡啶并[3,2-D]嘧啶-2,4(1H,3H)-二酮收率 248.1%

试剂、催化剂与溶剂 1

HCID 313盐酸溶剂

实验过程

20 g of 5-aminouracil (40 mmol), 80 ml of 20% HCl and 4 ml of crotonaldehyde (50 mmol) were heated together under reflux for 1 hour. The solution was evaporated to dryness under rotarary evaporation. Water was added to the residue so as to make the mixture just stirtable and then it was triturated with ammonium hydroxide with strong stirring until the pH increased to 10-11. Stirring was continued for another 10 minutes. The precipitate was filtered and was washed with minimal methanol and then chloroform and dried to give 17.58 g (63%) of 1.

后处理

  1. temperatureunder reflux for 1 hour
  2. customThe solution was evaporated to dryness under rotarary evaporation
  3. additionWater was added to the residue so as
  4. customit was triturated with ammonium hydroxide
  5. temperatureincreased to 10-11
  6. stirringStirring
  7. filtrationThe precipitate was filtered
  8. washwas washed with minimal methanol
  9. dry with materialchloroform and dried

来源与证据

ORD记录
ord-d399bb8e119f4bbab7a91306df8da12f
来源数据集
uspto-grants-1998_04
专利号
US05736547

反应笔记

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