تفاعل #444794

ord-49201b4bfa3b450eb7297845e60a5674

المذيبات

ظروف التفاعل

درجة الحرارة
120°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةCooling to room temperature
  2. 2
    ترشيحfiltration
  3. 3
    غسيلwashing the crystallizate with isopropanol
  4. 4
    أخرىdrying under a high vacuum

الإجراء التجريبي

20 ml of concentrated hydrochloric acid are added, with stirring, to a mixture of 5.09 g (0.0248 mol) of 4-(N-hydroxyamidino)-2,3-dihydro-1H-inden-1-one oxime, 6.23 g (0.0248 mol) of 1,2-diamino-4-(4-biphenylyl)-imidazole and 70 ml of isopropanol, and the mixture is stirred at 120° C. for 28 hours. Cooling to room temperature, filtration, washing the crystallizate with isopropanol and drying under a high vacuum yield the title compound with a water content of 0.9%, m.p. 284°-285° C. (decomp.), 1H-NMR (DMSO/D2O): δ=8.28 (d, 1H); 7.99 (s, 4H); 7.80 (s, 4H); 7.60-7.76 (m, 4H); 7.35-7.53 (m, 3H); 3.32 (s, 4H).

المصدر

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