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HCID 14081589, 화합물 → 2-(3-Amino-phenylmethanesulfonyl)-ethanol

HRID 2088724
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HRID 2088724 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([CH2:10][S:11]([CH2:14][CH2:15][OH:16])(=[O:13])=[O:12])[CH:7]=[CH:8][CH:9]=1)([O-])=O.[H][H]>CO.[Ni]>[NH2:1][C:4]1[CH:5]=[C:6]([CH2:10][S:11]([CH2:14][CH2:15][OH:16])(=[O:13])=[O:12])[CH:7]=[CH:8][CH:9]=1
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참가 물질

5

반응물 2

HCID 14081589HCID 14081589, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 153460102-(3-Amino-phenylmethanesulfonyl)-ethanol수율 73%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

2-(3-Nitro-phenylmethanesulfonyl)-ethanol (0.8 g, 3.3 mmol) (Harms, Wolfgang et al., Ger. Offen. (1995), DE 4402189 A1, 19950727) was placed in a hydrogenation flask and dissolved in methanol (100 mL). After the addition of Raney-Ni (200 mg) the mixture was allowed to shake at a hydrogen pressure of 70 psi at 50° C. for 4 hours. Then the catalyst was removed by filtration and washed with methanol. The methanol solutions were combined and the solvent evaporated under reduced pressure. The crude product was purified by flash-chromatography (eluent system: dichloromethane/methanol—10/1), the desired fractions were combined, dried and evaporated. The residue was washed with diethylether to afford 2-(3-amino-phenylmethanesulfonyl)-ethanol (0.51 g, yield 73%).

후처리

  1. customThen the catalyst was removed by filtration
  2. washwashed with methanol
  3. customthe solvent evaporated under reduced pressure
  4. customThe crude product was purified by flash-chromatography (eluent system: dichloromethane/methanol—10/1)
  5. customdried
  6. customevaporated
  7. washThe residue was washed with diethylether

출처 및 근거

ORD 기록
ord-ea8c11cbb88e4d53aead14c72976bc32
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08436007B2

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