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1-[4-(N-hydroxyamidino)-2,3-dihydro-1H-inden-1-ylideneamino]-2-amino-4-(4-methoxyphenyl)-imidazole dihydrochloride → 1-[4-(Amidino)-2,3-dihydro-1H-inden-1-ylideneamino]-2-amino-4-(4-methoxvphenyl)-imidazole dihydrochloride

HRID 357592
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인쇄 미리보기

반응식

HRID 357592 반응식
[ClH:1].Cl.O[NH:4][C:5]([C:7]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:8]=1[CH2:9][CH2:10][C:11]2=[N:16][N:17]1[CH:21]=[C:20]([C:22]2[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[CH:24][CH:23]=2)[N:19]=[C:18]1[NH2:30])=[NH:6]>[Ni].CO>[ClH:1].[ClH:1].[C:5]([C:7]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:8]=1[CH2:9][CH2:10][C:11]2=[N:16][N:17]1[CH:21]=[C:20]([C:22]2[CH:23]=[CH:24][C:25]([O:28][CH3:29])=[CH:26][CH:27]=2)[N:19]=[C:18]1[NH2:30])(=[NH:4])[NH2:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 1784887961-[4-(N-hydroxyamidino)-2,3-dihydro-1H-inden-1-ylideneamino]-2-amino-4-(4-methoxyphenyl)-imidazole dihydrochloride

생성물 1

HCID 699043811-[4-(Amidino)-2,3-dihydro-1H-inden-1-ylideneamino]-2-amino-4-(4-methoxvphenyl)-imidazole dihydrochloride

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

Analogously to Example 2, approximately 2 g of Raney nickel are added to a solution of 5.8 g (0.00129 mol) of 1-[4-(N-hydroxyamidino)-2,3-dihydro-1H-inden-1-ylideneamino]-2-amino-4-(4-methoxyphenyl)-imidazole dihydrochloride in 600 ml of methanol, and hydrogenation is carried out at room temperature and under normal pressure until the absorption of hydrogen has ceased. The reaction mixture is then filtered and the filtrate is concentrated. The product that has crystallised out is filtered off with suction and recrystallized from methanol, yielding the title compound in the form of the monohydrate, m.p. >220° C., 1H-NMR (DMSO): δ=9.56 (d, 4H); 8.33 (d, 1H); 7.99 (s, 1H); 7.94 (s, 2H); 7.75-7.84 (m, 3H); 7.64 (t, 1H); 7.04 (d, 2H); 3.80 (s, 3H), 3.40 (m, 4H).

후처리

  1. customis carried out at room temperature and under normal pressure until the absorption of hydrogen
  2. filtrationThe reaction mixture is then filtered
  3. concentrationthe filtrate is concentrated
  4. customThe product that has crystallised out
  5. filtrationis filtered off with suction
  6. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-c23f041aa4ca4f4daeed647d7eb75156
출처 데이터셋
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05840911

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