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 70811노트

반응식

HRID 70811 반응식
[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]

참가 물질

4

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-49fef30d9315451796e4194dd8f8f7a7
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822691B2

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