2,3-Dibromobutane → HCID 67171497, 화합물

HRID 551115

반응식

HRID 551115 반응식
[NH2:1][C:2]1[CH:11]=[C:10]([CH:12]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[NH:13][C:14](=[O:23])[CH2:15][O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:9]([OH:30])=[C:8]2[C:3]=1[CH:4]=[CH:5][CH:6]=[N:7]2.Br[CH:32]([CH:34](Br)[CH3:35])[CH3:33]>C(O)(C)C>[OH:30][C:9]1[C:10]([CH:12]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[NH:13][C:14](=[O:23])[CH2:15][O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:11][C:2]([N:1]2[CH2:35][CH2:34][CH2:32][CH2:33]2)=[C:3]2[C:8]=1[N:7]=[CH:6][CH:5]=[CH:4]2

참가 물질

4

반응물 2

HCID 215082,3-DibromobutaneHCID 67171864HCID 67171864, 화합물

생성물 1

HCID 67171497HCID 67171497, 화합물

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

N-[(5-amino-8-hydroxyquinolin-7-yl)(phenyl)methyl]-2-phenoxyacetamide (200 mg, 0.5 mmol), dibromobutane (0.1 ml), TEA (0.2 ml) in isopropanol were heated at reflux for 16 h. The reaction mixture was concentrated in vacuo, the residue dissolved in methylene chloride, washed with brine. The organic layer was dried over sodium sulfate and filtered. To the filtrate was added 1M HCl/ether, the solids filtered, washed with ether to give N-[(8-hydroxy-5-pyrrolidin-1-ylquinolin-7-yl)(phenyl)methyl]-2-phenoxyacetamide as a purple solid.

후처리

  1. temperatureat reflux for 16 h
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. dissolutionthe residue dissolved in methylene chloride
  4. washwashed with brine
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. filtrationfiltered
  7. additionTo the filtrate was added 1M HCl/ether
  8. filtrationthe solids filtered
  9. washwashed with ether

출처 및 근거

ORD 기록
ord-991e57e57f2646bb808f4e3c5d032f66
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07947712B2

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