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

HRID 1194019

反応式

HRID 1194019 の反応式
[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]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 124801-PhenylpyrroleHCID 167232,4,5,6(1H,3H)-Pyrimidinetetrone, monohydrate2 回

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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) was 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)].

後処理

  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

出典と根拠

ORDレコード
ord-5e54170925304ed693f7ed2f55ac55e4
出典データセット
uspto-grants-1989_03
特許番号
US04812471

関連ノート

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