p-Toluenesulfonic acid → 1-[4-(Amidino)-2,3-dihydro-1H-inden-1-ylideneamino]-2-amino-4,5-di-hydro-imidazole dihydrochloride

HRID 357621

反応式

HRID 357621 の反応式
[ClH:1].[C:2]([C:5]1[CH:13]=[CH:12][CH:11]=[C:10]2[C:6]=1[CH2:7][CH2:8][C:9]2=O)(=[NH:4])[NH2:3].Cl.[NH2:16][N:17]1[CH2:21][CH2:20][N:19]=[C:18]1[NH2:22].CC1C=CC(S(O)(=O)=O)=CC=1.C=CC1C=CC=CC=1.C(C1C=CC=CC=1C=C)=C>O>[ClH:1].[ClH:1].[C:2]([C:5]1[CH:13]=[CH:12][CH:11]=[C:10]2[C:6]=1[CH2:7][CH2:8][C:9]2=[N:16][N:17]1[CH2:21][CH2:20][N:19]=[C:18]1[NH2:22])(=[NH:4])[NH2:3]

参加物

6

反応物 4

HCID 6101p-Toluenesulfonic acidHCID 174664Divinylbenzene-styreneHCID 189379401,2-Diamino-4,5-dihydro-imidazole hydrochlorideHCID 189379431-Oxo-2,3-dihydro-1H-indene-4-carboximidamide--hydrogen chloride (1/1)

生成物 1

HCID 699043851-[4-(Amidino)-2,3-dihydro-1H-inden-1-ylideneamino]-2-amino-4,5-di-hydro-imidazole dihydrochloride

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 0.24 g (0.001 mol) of 4-amidino-2,3-dihydro-1H-inden-1-one hydrochloride and 0.136 g (0.001 mol) of 1,2-diamino-4,5-dihydro-imidazole hydrochloride [m.p. 245°-246° C., prepared from the corresponding p-toluenesulfonate salt, see EP 0 327 919, Example 12, by ion exchange on ®Amberlite IRA-400 (anion exchanger based on a styrene/divinylbenzene polymer with quaternary ammonium groups in the Cl- form; Fluka, Buchs, Switzerland)] in 3 ml of water is left to stand at room temperature for 18 hours. The product that has crystallized out is filtered off with suction and recrystallized from water, yielding the title compound (monohydrate), m.p. 280° C. (decomp.), 1 H-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

  1. customThe product that has crystallized out
  2. filtrationis filtered off with suction
  3. customrecrystallized from water

出典と根拠

ORDレコード
ord-97b2d694d9664a8eaae5ae32eeeca138
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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