Chlorosuccinimide → HCID 85444714, 화합물

HRID 1173259노트

반응식

HRID 1173259 반응식
[F:1][C:2]([F:13])([F:12])[C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][CH:11]=1)[CH:6]=[N:7][OH:8].[Cl:14]N1C(=O)CCC1=O>C(Cl)Cl.O>[OH:8][N:7]=[C:6]([Cl:14])[C:5]1[CH:9]=[CH:10][CH:11]=[C:3]([C:2]([F:12])([F:13])[F:1])[CH:4]=1

참가 물질

5

반응물 2

HCID 31398ChlorosuccinimideHCID 2777383N-{[3-(Trifluoromethyl)phenyl]methylidene}hydroxylamine

생성물 1

HCID 85444714HCID 85444714, 화합물수율 90%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

반응 조건

온도
45 °C

실험 절차

To a dried flask containing 3-(trifluoromethyl)benzaldehyde oxime (1.89 g, 10 mol) in methylene chloride (100 mL) was added N-chlorosuccinimide (1.40 g, 10.5 mmol) slowly at 0° C. The reaction mixture was warmed to 45° C. for 2 h, poured over ice, diluted with H2O (20 mL), and extracted with EtOAc (100 mL). The organic phase was washed with H2O (2×25 mL) and saline solution (25 mL), dried over sodium sulfate, concentrated in vacuo to give N-hydroxy -3-(trifluoromethyl)benzenecarboximidoyl chloride (2 g, 90% o). LCMS: 224.4 (M+H)+.

후처리

  1. additionpoured over ice
  2. extractionextracted with EtOAc (100 mL)
  3. washThe organic phase was washed with H2O (2×25 mL) and saline solution (25 mL)
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-ff14b033cb0c4896b380bfbfd3ab441c
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07834021B2

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