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[2-(5-Benzylamino-3-bromo-4-nitropyrazol-1-yl)ethyl]carbamic acid tert-butyl ester → Hydrogen Bromide

HRID 1744174
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HRID 1744174 반응식
[C:1]([O:5][C:6](=[O:27])[NH:7][CH2:8][CH2:9][N:10]1[C:14]([NH:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[C:13]([N+:23]([O-:25])=[O:24])[C:12]([Br:26])=[N:11]1)([CH3:4])([CH3:3])[CH3:2]>CCO.[Pd]>[C:1]([O:5][C:6](=[O:27])[NH:7][CH2:8][CH2:9][N:10]1[C:14]([NH:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[C:13]([N+:23]([O-:25])=[O:24])[C:12]([Br:26])=[N:11]1)([CH3:4])([CH3:2])[CH3:3].[BrH:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

HCID 13007947[2-(5-Benzylamino-3-bromo-4-nitropyrazol-1-yl)ethyl]carbamic acid tert-butyl ester

생성물 2

HCID 260Hydrogen BromideHCID 13007947[2-(5-Benzylamino-3-bromo-4-nitropyrazol-1-yl)ethyl]carbamic acid tert-butyl ester

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

A mixture of [2-(5-benzylamino-3-bromo-4-nitropyrazol-1-yl)ethyl]carbamic acid tert-butyl ester (2.1 g; 4.76 mmol) in EtOH (100 ml) containing a 5% Pd/C catalyst (Engelhard type, 50% moisture, 0.4 g wet weight) was hydrogenated in an autoclave (250 ml) at 15 bar for 3 h. The catalyst was filtered off under an inert atmosphere and washed with EtOH, and the filtrate was recovered in an ethanolic solution (25 ml) containing hydrobromic acid (47%, 2 ml). The orange-colored solution was evaporated to dryness to give the 2-(2-aminoethyl)-2H-pyrazole-3,4-diamine in the hydrobromide form (3.55 HBr) as a pale pink solid (1.5 g, 92%).

후처리

  1. filtrationThe catalyst was filtered off under an inert atmosphere
  2. washwashed with EtOH
  3. customthe filtrate was recovered in an ethanolic solution (25 ml)
  4. additioncontaining hydrobromic acid (47%, 2 ml)
  5. customThe orange-colored solution was evaporated to dryness

출처 및 근거

ORD 기록
ord-de7d0c6c8bdf4353abfbfdc14eb20a86
출처 데이터셋
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07014663B2

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