m-Chloroperbenzoic acid → N-[2-Bromo-4-(1-bromo-1,1,2,3,3,3-hexafluoropropan-2-yl)-6-(difluoromethoxy)phenyl]-quinoline-6-carboxamide-1-oxide

HRID 70811ノート

反応式

HRID 70811 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([C:8]([F:17])([C:13]([F:16])([F:15])[F:14])[C:9]([Br:12])([F:11])[F:10])[CH:5]=[C:4]([O:18][CH:19]([F:21])[F:20])[C:3]=1[NH:22][C:23]([C:25]1[CH:26]=[C:27]2[C:32](=[CH:33][CH:34]=1)[N:31]=[CH:30][CH:29]=[CH:28]2)=[O:24].ClC1C=CC=C(C(OO)=[O:43])C=1>ClCCl>[Br:1][C:2]1[CH:7]=[C:6]([C:8]([F:17])([C:13]([F:15])([F:14])[F:16])[C:9]([Br:12])([F:10])[F:11])[CH:5]=[C:4]([O:18][CH:19]([F:20])[F:21])[C:3]=1[NH:22][C:23]([C:25]1[CH:26]=[C:27]2[C:32](=[CH:33][CH:34]=1)[N+:31]([O-:43])=[CH:30][CH:29]=[CH:28]2)=[O:24]

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 86672969N-[2-Bromo-4-(1-bromo-1,1,2,3,3,3-hexafluoropropan-2-yl)-6-(difluoromethoxy)phenyl]-quinoline-6-carboxamide

生成物 1

HCID 86672968N-[2-Bromo-4-(1-bromo-1,1,2,3,3,3-hexafluoropropan-2-yl)-6-(difluoromethoxy)phenyl]-quinoline-6-carboxamide-1-oxide収率 108.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

N-[2-Bromo-4-(1-bromo-1,1,2,3,3,3-hexafluoropropan-2-yl)-6-(difluoromethoxy)phenyl]-quinoline-6-carboxamide (0.73 g) was dissolved in dichloromethane (50 ml), added with 3-chloroperbenzoic acid (purity 70%, 0.48 g), and sited at room temperature for S hours. The solvent was distilled off under the reduced pressure and the residue was dissolved in ethyl acetate, Sodium hydrocarbonate solution and potassium carbonate were added thereto. After extracting the mixture twice with ethyl acetate, the organic phases were combined and washed with water, and dried over anhydrous magnesium sulfate. The drying agent (anhydrous magnesium sulfate) was filtered off and the solvent was removed by distillation under the 1.5 reduced pressure to obtain N-[2-bromo-4-(1-bromo-1,1,2,3,3,3-hexafluoropropan-2-yl)-6-(difluoromethoxy)phenyl]quinoline-6-carboxamide-1-oxide (0.81 g, 98%).

後処理

  1. customsited at room temperature for S hours
  2. distillationThe solvent was distilled off under the reduced pressure
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. additionSodium hydrocarbonate solution and potassium carbonate were added
  5. extractionAfter extracting the mixture twice with ethyl acetate
  6. washwashed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationThe drying agent (anhydrous magnesium sulfate) was filtered off
  9. customthe solvent was removed by distillation under the 1.5 reduced pressure

出典と根拠

ORDレコード
ord-49fef30d9315451796e4194dd8f8f7a7
出典データセット
uspto-grants-2014_09
特許番号
US08822691B2

反応ノート

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