海萝胶 → 5-Hydroxy-5-(1-phenyl-2-pyrrolyl)-2,4,6-(1H,3H,5H)pyrimidinetrione

HRID 1388522

反应方程式

HRID 1388522 反应方程式
[C:1]1([N:7]2[CH:11]=[CH:10][CH:9]=[CH:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.[NH:13]1[C:21](=[O:22])[C:19](=[O:20])[C:17](=[O:18])[NH:16][C:14]1=[O:15].Cl>C(O)C>[OH:20][C:19]1([C:8]2[N:7]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[CH:11]=[CH:10][CH:9]=2)[C:17](=[O:18])[NH:16][C:14](=[O:15])[NH:13][C:21]1=[O:22]

参与物

5

反应物 3

HCID 313海萝胶HCID 124801-苯基吡咯HCID 16723阿脲一水合物2 次

产物 1

HCID 132828945-Hydroxy-5-(1-phenyl-2-pyrrolyl)-2,4,6-(1H,3H,5H)pyrimidinetrione收率 80.6%

试剂、催化剂与溶剂 1

HCID 702乙醇溶剂

实验过程

1-Phenylpyrrole (1.4 g., 0.01 mole), alloxan hydrate (1.6 g., 0.01 mole) and 50 ml. of ethanol were combined and refluxed for 15 minutes. No reaction was noted by tlc. 1N Hydrochloric acid (10 ml., 0.01 mole) added and the acidified mixture refluxed for 15 minutes. Incomplete reaction was noted by tlc. A second portion of alloxan hydrate (1.6 g., 0.01 mole) was added and the mixture refluxed another 15 minutes, cooled and evaporated to dryness. Trituration of the residue with water gave title product [2.3 g.; m/e 285; m.p. 232°-234° C. (dec); Rf 0.3 (1:1 ethyl acetate:hexane)].

后处理

  1. temperaturerefluxed for 15 minutes
  2. temperaturethe acidified mixture refluxed for 15 minutes
  3. customIncomplete reaction
  4. temperaturethe mixture refluxed another 15 minutes
  5. temperaturecooled
  6. customevaporated to dryness

来源与证据

ORD记录
ord-8c3162f71b6b44d59ced50aad17edc66
来源数据集
uspto-grants-1984_02
专利号
US04431810

关联笔记

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