Urea → 3-Methyl-4-hydroxy-4-ureidocarbonyl-2-oxo-1,2,3,4-tetrahydroquinazoline

HRID 34553

反応式

HRID 34553 の反応式
[CH3:1][NH:2][C:3]([N:5]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:8](=[O:9])[C:6]1=[O:7])=[O:4].C1CCN2C(=NCCC2)CC1.[NH2:27][C:28]([NH2:30])=[O:29]>O1CCCC1>[CH3:1][N:2]1[C:8]([OH:9])([C:6]([NH:27][C:28]([NH2:30])=[O:29])=[O:7])[C:10]2[C:15](=[CH:14][CH:13]=[CH:12][CH:11]=2)[NH:5][C:3]1=[O:4]

参加物

5

反応物 3

HCID 1176UreaHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 2835543N-(methylcarbamoyl)isatin

生成物 1

HCID 142299933-Methyl-4-hydroxy-4-ureidocarbonyl-2-oxo-1,2,3,4-tetrahydroquinazoline

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

1-Methylcarbamoylisatin (10.2 g) and 1,8-diazabicyclo[5.4.0]-7-undecene (0.3 g) are dissolved in tetrahydrofuran (100 ml), and thereto is added urea (4.5 g), and the mixture is refluxed for 10 hours. After cooling, the precipitates are taken by filtration, washed with water and methanol and recrystallized from a mixture of dimethylsulfoxide and ethanol to give 3-methyl-4-hydroxy-4-ureidocarbonyl-2-oxo-1,2,3,4-tetrahydroquinazoline, M.p.>280° C.,

後処理

  1. temperaturethe mixture is refluxed for 10 hours
  2. temperatureAfter cooling
  3. filtrationthe precipitates are taken by filtration
  4. washwashed with water and methanol
  5. customrecrystallized from a mixture of dimethylsulfoxide and ethanol

出典と根拠

ORDレコード
ord-ee11b7a4037446ff838830f2b1b77ab6
出典データセット
uspto-grants-1988_08
特許番号
US04762839

関連ノート

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