2,3-Dibromobutane → HCID 67171497、化合物

HRID 551115

反応式

HRID 551115 の反応式
[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

参加物

4

反応物 2

HCID 215082,3-DibromobutaneHCID 67171864HCID 67171864、化合物

生成物 1

HCID 67171497HCID 67171497、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-991e57e57f2646bb808f4e3c5d032f66
出典データセット
uspto-grants-2011_05
特許番号
US07947712B2

関連ノート

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