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

HRID 357621

반응식

HRID 357621 반응식
[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]

참가 물질

6

반응물 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)

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-97b2d694d9664a8eaae5ae32eeeca138
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840911

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