Hydrochloric Acid → HCID 178478845、化合物

HRID 357610

反応式

HRID 357610 の反応式
[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]

参加物

7

反応物 5

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

生成物 1

HCID 178478845HCID 178478845、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-baf3b5216d004be2abe28a39dc27158b
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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