反応式
[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[CH2:21][CH2:20][N:19]=[C:18]1[NH2:22])=[NH:6]>[Ni].O>[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[CH2:21][CH2:20][N:19]=[C:18]1[NH2:22])(=[NH:4])[NH2:6]参加物
実験手順
Analogously to Example 2, approximately 2.0 g of Raney nickel are added to a solution of 4.75 g (0.0138 mol) of 1-[4-(N-hydroxyamidino)-2,3-dihydro-1H-inden-1-ylideneamino]-2-amino-4,5-dihydro-imidazole dihydrochloride in 240 ml of water, 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, adjusted to pH 4 with a small amount of 2N alcoholic hydrochloric acid and concentrated to dryness by evaporation. The residue is recrystallized from water, yielding the title compound in the form of the monohydrate, m.p. 280° C. (decomp.), 1H-NMR (DMSO/D2O): δ=8.17 (d, 1H); 7.66 (d, 1H); 7.54 (t, 1H); 4.18 (t, 2H); 3.70 (t, 2H); 3.25 (m, 2H); 3.13 (m, 2H).
後処理
- customis carried out at room temperature and under normal pressure until the absorption of hydrogen
- filtrationThe reaction mixture is then filtered
- concentrationconcentrated to dryness by evaporation
- customThe residue is recrystallized from water
出典と根拠
- ORDレコード
- ord-3d0783ad72a14ddf96c3ca397da557a8
- 出典データセット
- uspto-grants-1998_11
- 特許番号
- US05840911
関連ノート
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