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

HRID 508447
ノート
印刷プレビュー

反応式

HRID 508447 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 679
Dimethyl Sulfoxide
溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-26e32dd0d1a54eea980f081ad77e1cf6
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09096500B2

反応ノート

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