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1,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene) → Methyl 8-bromo-4-oxo-1,4-dihydroquinoline-6-carboxylate

HRID 1778263
ノート
印刷プレビュー

反応式

HRID 1778263 の反応式
C1C=CC(C2C=CC=CC=2)=CC=1.C1C=CC(OC2C=CC=CC=2)=CC=1.[Br:26][C:27]1[CH:28]=[C:29]([CH:34]=[CH:35][C:36]=1[NH:37][CH:38]=[C:39]1[C:44](=[O:45])OC(C)(C)OC1=O)[C:30]([O:32][CH3:33])=[O:31]>>[Br:26][C:27]1[CH:28]=[C:29]([C:30]([O:32][CH3:33])=[O:31])[CH:34]=[C:35]2[C:36]=1[NH:37][CH:38]=[CH:39][C:44]2=[O:45]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 246701,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene)HCID 118323992Methyl 3-bromo-4-(((2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-ylidene)methyl)amino)benzoate

生成物 1

HCID 118324114Methyl 8-bromo-4-oxo-1,4-dihydroquinoline-6-carboxylate

実験手順

To a flask with DOWTHERM (35 mL) at 210° C. was added methyl 3-bromo-4-(((2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-ylidene)methyl)amino)benzoate (3.3 g, 8.59 mmol) in portions. The resulting solution was heated for 20 min and cooled down to room temperature. Solids were precipitated from the solution. To the reaction mixture was then added hexanes and the precipitate filtered. The solids were washed thoroughly with Et2O and hexanes and dried under vacuum to yield methyl 8-bromo-4-oxo-1,4-dihydroquinoline-6-carboxylate. (M+H)+: 282, 284

後処理

temperature
The resulting solution was heated for 20 min
  • customSolids were precipitated from the solution
  • filtrationadded hexanes and the precipitate filtered
  • washThe solids were washed thoroughly with Et2O and hexanes
  • customdried under vacuum
  • 出典と根拠

    ORDレコード
    ord-28498b60af3b45e889b0270398358159
    出典データセット
    uspto-grants-2016_02
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US09266835B2

    反応ノート

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