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Hydrazine → tert-Butyl 2-[(2-Aminophenyl)amino]ethylcarbamate

HRID 1984538
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HRID 1984538 반응식
[C:1]([O:5][C:6](=[O:20])[NH:7][CH2:8][CH2:9][NH:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[N+:17]([O-])=O)([CH3:4])([CH3:3])[CH3:2].NN.[O-]S([O-])(=O)=O.[Mg+2]>CO.[Ni]>[C:1]([O:5][C:6](=[O:20])[NH:7][CH2:8][CH2:9][NH:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[NH2:17])([CH3:4])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 9321HydrazineHCID 24083Sulfuric acid magnesium salt (1:1)HCID 47453724tert-Butyl 2-(2-nitrophenylamino)ethylcarbamate

생성물 1

HCID 28875325tert-Butyl 2-[(2-Aminophenyl)amino]ethylcarbamate수율 72%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887
Methanol
용매

실험 절차

A mixture of [2-(2-nitrophenylamino)ethyl]carbamic acid t-butyl ester (6 g, 21.3 mmol) and Raney-Nickel (0.5 g) in methanol is treated dropwise with hydrazine (0.8 mL, 25 mmol), stirred at room temperature until reaction is complete by TLC, treated with Celite and MgSO4 and filtered. The filtercake is washed with methanol. The filtrates are combined and concentrated in vacuo to give the title compound as a brown oil, 3.85 g (72% yield), identified by HPLC and mass spectral analyses.

후처리

  1. filtrationfiltered
  2. washThe filtercake is washed with methanol
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-a578f7ac6d2c41a4aacfa81cfa3169ba
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07544701B2

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