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Tert-butyl 4-(3-methoxy-4-nitrophenyl)piperazine-1-carboxylate → Tert-butyl 4-(4-amino-3-methoxyphenyl)piperazine-1-carboxylate

HRID 1503813
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인쇄 미리보기

반응식

HRID 1503813 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([N:12]2[CH2:17][CH2:16][N:15]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:14][CH2:13]2)[CH:6]=[CH:7][C:8]=1[N+:9]([O-])=O>[Ni].CO>[NH2:9][C:8]1[CH:7]=[CH:6][C:5]([N:12]2[CH2:17][CH2:16][N:15]([C:18]([O:20][C:21]([CH3:22])([CH3:23])[CH3:24])=[O:19])[CH2:14][CH2:13]2)=[CH:4][C:3]=1[O:2][CH3:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 25918710Tert-butyl 4-(3-methoxy-4-nitrophenyl)piperazine-1-carboxylate

생성물 1

HCID 67128946Tert-butyl 4-(4-amino-3-methoxyphenyl)piperazine-1-carboxylate

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

A suspension of the product of Example 13A (6.3 g, 18.7 mmol) and Raney nickel (2.0 g) in 300 mL methanol was stirred under hydrogen at ambient temperature for 5 hours. The mixture was filtered through diatomaceous earth and the filtrate was concentrated. The residue was purified by flash chromatography on silica gel (200-300 mesh) eluting with a gradient of 2/1 to 1/1 petroleum/ethyl acetate to give the title compound.

후처리

  1. filtrationThe mixture was filtered through diatomaceous earth
  2. concentrationthe filtrate was concentrated
  3. customThe residue was purified by flash chromatography on silica gel (200-300 mesh)
  4. washeluting with a gradient of 2/1 to 1/1 petroleum/ethyl acetate

출처 및 근거

ORD 기록
ord-c1c8820c536b408fac6aebf9a2452163
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09212192B2

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