Hydrochloric Acid → HCID 178478845, 화합물

HRID 357610

반응식

HRID 357610 반응식
[ClH:1].[OH:2][NH:3][C:4]([C:6]1[CH:14]=[CH:13][CH:12]=[C:11]2[C:7]=1[CH2:8][CH2:9][C:10]2=[N:15]O)=[NH:5].Cl.N[N:19]1[CH2:23][CH2:22][N:21]=[C:20]1[NH2:24].CC1C=CC(S(O)(=O)=O)=CC=1.C=CC1C=CC=CC=1.C(C1C=CC=CC=1C=C)=C>C(O)(C)C>[ClH:1].[ClH:1].[OH:2][NH:3][C:4]([C:6]1[CH:14]=[CH:13][CH:12]=[C:11]2[C:7]=1[CH2:8][CH2:9][C:10]2=[N:15][N:21]1[CH2:22][CH2:23][N:19]=[C:20]1[NH2:24])=[NH:5]

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 6101p-Toluenesulfonic acidHCID 174664Divinylbenzene-styreneHCID 189379401,2-Diamino-4,5-dihydro-imidazole hydrochlorideHCID 178513250HCID 178513250, 화합물

생성물 1

HCID 178478845HCID 178478845, 화합물

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

0.5 ml of 32% hydrochloric acid (Merck, Darmstadt, Germany; p.a.) is added, with stirring, to a mixture of 0.51 g (0.0025 mol) of 4-(N-hydroxyamidino)-2,3-dihydro-1H-inden-1-one oxime, 0.342 g (0.0025 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)] and 12 ml of isopropanol, and the reaction mixture is stirred at 80°-90° C. for 16 hours. The reaction mixture is filtered while hot and the filtration product is washed with isopropanol and recrystallized from hot water. In that manner there is obtained the title compound, m.p. >245° C., 1H-NMR (D2O): δ=8.08 (d, 1H); 7.72 (d, 1H); 7.56 (t, 1H); 4.14 (t, 2H); 3.81 (t, 2H); 3.3 (m, 2H); 3.15 (m, 2H).

후처리

  1. filtrationThe reaction mixture is filtered while hot and the filtration product
  2. washis washed with isopropanol
  3. customrecrystallized from hot water

출처 및 근거

ORD 기록
ord-baf3b5216d004be2abe28a39dc27158b
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840911

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