تفاعل #444785

ord-d5fe3f14e48245f5ad98cb4755ed10da

ظروف التفاعل

درجة الحرارة
110°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزis then concentrated in vacuo to approximately half its original volume
  2. 2
    أخرىThe product that has crystallized out
  3. 3
    ترشيحis filtered off
  4. 4
    غسيلwashed with isopropanol
  5. 5
    أخرىrecrystallized from a mixture of 15 ml of methanol and 30 ml of isopropanol

الإجراء التجريبي

A mixture of 1.20 g (5.848 mmol) of 4-(N-hydroxyamidino)-2,3-dihydro-1H-inden-1-one oxime, 1.10 g (5.844 mmol) of 1,2-diamino-4-(4-tolyl)-imidazole (Beyer H. et al., Chem. Ber. 101, 3151 (1968)) and 20 ml of 4N hydrochloric acid is heated at 110° C. for 22 hours, with stirring, and is then concentrated in vacuo to approximately half its original volume. The product that has crystallized out is filtered off, washed with isopropanol and recrystallized from a mixture of 15 ml of methanol and 30 ml of isopropanol, yielding the title compound in the form of the dihydrate, m.p. 225°-232° C. (decomp.), 1H-NMR (D2O): δ=8.04 (d, 1H); 7.74 (d, 1H); 7.55 (t, 1H); 7.30 (s, 1H); 7.26 (d, 2H); 7.07 (d, 2H); 3.17-3.23 (m, 2H); 2.98-3.04 (m, 2H); 2.07 (s, 3H).

المصدر

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