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Hydrogen Peroxide → 2,5-Difluoro-4-[4-chloro-3-(trifluoromethyl)phenylmethoxy]-benzamide

HRID 508447
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HRID 508447 반응식
[F:1][C:2]1[CH:9]=[C:8]([O:10][CH2:11][C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([C:19]([F:22])([F:21])[F:20])[CH:13]=2)[C:7]([F:23])=[CH:6][C:3]=1[C:4]#[N:5].C(=O)([O-])[O-:25].[K+].[K+].OO.O>CS(C)=O>[F:1][C:2]1[CH:9]=[C:8]([O:10][CH2:11][C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([C:19]([F:20])([F:22])[F:21])[CH:13]=2)[C:7]([F:23])=[CH:6][C:3]=1[C:4]([NH2:5])=[O:25]
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참가 물질

6

반응물 4

HCID 784Hydrogen PeroxideHCID 962WaterHCID 11430Potassium CarbonateHCID 866825572,5-Difluoro-4-[4-chloro-3-(trifluoromethyl)phenylmethoxy]-benzonitrile

생성물 1

HCID 866825582,5-Difluoro-4-[4-chloro-3-(trifluoromethyl)phenylmethoxy]-benzamide수율 87.5%

시약·촉매·용매 1

HCID 679
Dimethyl Sulfoxide
용매

실험 절차

To a suspension of 2,5-difluoro-4-[4-chloro-3-(trifluoromethyl)phenylmethoxy]-benzonitrile (Preparation 61, 0.2 g, 0.5 mmol) and potassium carbonate (0.39 g, 2.5 mmol) in DMSO (3 mL), was added hydrogen peroxide (30% solution in water, 0.6 mL, 5 mmol) at room temperature. The resulting mixture was stirred for 3 hours at room temperature. Water (30 mL) was then added and the precipitate formed was filtered. The filtrate was extracted twice with EtOAc and combined with the solid. The resulting organic solution was dried over magnesium sulphate, filtered and evaporated to afford the title compound as a white solid (160 mg, 76%).

후처리

  1. customthe precipitate formed
  2. filtrationwas filtered
  3. extractionThe filtrate was extracted twice with EtOAc
  4. dry with materialThe resulting organic solution was dried over magnesium sulphate
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-26e32dd0d1a54eea980f081ad77e1cf6
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09096500B2

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