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

HRID 34553

반응식

HRID 34553 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.,

후처리

  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

출처 및 근거

ORD 기록
ord-ee11b7a4037446ff838830f2b1b77ab6
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04762839

연결된 노트

불러오는 중…