تفاعل #444774

ord-c23f041aa4ca4f4daeed647d7eb75156

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىis carried out at room temperature and under normal pressure until the absorption of hydrogen
  2. 2
    ترشيحThe reaction mixture is then filtered
  3. 3
    تركيزthe filtrate is concentrated
  4. 4
    أخرىThe product that has crystallised out
  5. 5
    ترشيحis filtered off with suction
  6. 6
    أخرىrecrystallized from methanol

الإجراء التجريبي

Analogously to Example 2, approximately 2 g of Raney nickel are added to a solution of 5.8 g (0.00129 mol) of 1-[4-(N-hydroxyamidino)-2,3-dihydro-1H-inden-1-ylideneamino]-2-amino-4-(4-methoxyphenyl)-imidazole dihydrochloride in 600 ml of methanol, 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 and the filtrate is concentrated. The product that has crystallised out is filtered off with suction and recrystallized from methanol, yielding the title compound in the form of the monohydrate, m.p. >220° C., 1H-NMR (DMSO): δ=9.56 (d, 4H); 8.33 (d, 1H); 7.99 (s, 1H); 7.94 (s, 2H); 7.75-7.84 (m, 3H); 7.64 (t, 1H); 7.04 (d, 2H); 3.80 (s, 3H), 3.40 (m, 4H).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05840911uspto-grants-1998_11