Hydrogen Peroxide → 2-(2-Fluorophenyl)isobutyramide

HRID 736445

반응식

HRID 736445 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([CH3:12])([CH3:11])[C:9]#[N:10].[OH-:13].[Na+].OO>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.C1(C)C=CC=CC=1>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([CH3:12])([CH3:11])[C:9]([NH2:10])=[O:13]

참가 물질

6

반응물 3

HCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 119764412-(2-Fluorophenyl)-2-methylpropanenitrile

생성물 1

HCID 119764962-(2-Fluorophenyl)isobutyramide

시약·촉매·용매 2

HCID 94433Tetrabutylammonium hydrogen sulfate촉매HCID 1140Toluene용매

실험 절차

2-(2-Fluorophenyl)-2-methylpropionitrile (0.211 g) was magnetically stirred with aqueous solutions of 5N sodium hydroxide (2 mL), 55% tetrabutylammonium hydrogensulfate (0.1 mL) and 30% hydrogen peroxide (3 mL) for 22 hours. The reaction mixture was diluted with toluene and extracted. The aqueous phase was neutralized with 5% hydrochloric acid and extracted twice with ethyl acetate. The combined organic extracts were washed with water, then brine, and dried over anhydrous magnesium sulfate. Filtration and evaporation gave 2-(2-fluorophenyl)isobutyramide as a pale-green oil that solidified on standing (0.173 g). GC/MS: m/z 181 (RT 9.80 min.). 1H-NMR (DMSO-d6): 7.39-7.27 (m, 2H), 7.19-7.07 (m, 2H), 6.83 and 6.78 (2 s, CONH2), 1.43 (s, 6H)

후처리

  1. extractionextracted
  2. extractionextracted twice with ethyl acetate
  3. washThe combined organic extracts were washed with water
  4. dry with materialbrine, and dried over anhydrous magnesium sulfate
  5. filtrationFiltration and evaporation

출처 및 근거

ORD 기록
ord-efcc971d98ab4a76b3e31546f5e23bf2
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07595338B2

연결된 노트

불러오는 중…