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Acetic Anhydride → HCID 22386582, 화합물

HRID 1067491
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HRID 1067491 반응식
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][C:10]=2[O:12][C:13]2[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][CH:14]=2)[N:5]=[CH:4][N:3]=1.N1C=CC=CC=1.ClCCl.[C:30](OC(=O)C)(=[O:32])[CH3:31]>>[C:30]([NH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][C:10]=2[O:12][C:13]2[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][CH:14]=2)[N:5]=[CH:4][N:3]=1)(=[O:32])[CH3:31]
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참가 물질

4

반응물 3

HCID 7918Acetic AnhydrideHCID 21875418Pyridine methylene chlorideHCID 22386590HCID 22386590, 화합물

생성물 1

HCID 22386582HCID 22386582, 화합물수율 45.4%

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온도
4 °C

실험 절차

To a stirred solution of 4-amino-5-(4-methoxyphenoxy)quinazoline (1.0 g, 3.7 mmol) in 30 ml of dichloromethane pyridine (0.3 g, 3.7 mmol) and acetic anhydride (0.38 g, 3.7 mmol) were added at room temperature and stirring continued for 4 days. After evaporation under reduced pressure, 30 ml of 2-propanol was added and after cooling to 4° C. the solid was collected by filtration, washed, recrystallized from ethanol, filtrated again and dried at 50° C. in vacuo. to give 4-acetamido-5-(4methoxyphenoxy)quinazoline (0.5 g, 45.4%, m.p. 174-175° C.).

후처리

  1. customAfter evaporation under reduced pressure, 30 ml of 2-propanol
  2. additionwas added
  3. filtrationwas collected by filtration
  4. washwashed
  5. customrecrystallized from ethanol
  6. filtrationfiltrated again
  7. customdried at 50° C. in vacuo

출처 및 근거

ORD 기록
ord-a6389ff7668742f192eb69b5ce4e379d
출처 데이터셋
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06248771B1

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