تفاعل #342721

ord-0e2730d88efe48169e176305209b589a

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe mixture was heated at its
  2. 2
    درجة الحرارةreflux temperature for two hours
  3. 3
    أخرىEvaporation
  4. 4
    أخرىprovided a residue which
  5. 5
    أخرىseparated by filtration
  6. 6
    غسيلwashed with water
  7. 7
    أخرىRecrystallization from ethanol

الإجراء التجريبي

To a solution of 6.6 g (0.041 mole) of 3,4-diaminoquinoline (from Example 39), 2.0 ml of glacial acetic acid, 35 cc of ethanol and 35 ml of water was added 9.3 g (0.045 mole) of N-carbomethoxy-S-methylisothiourea, and the mixture was heated at its reflux temperature for two hours. Evaporation provided a residue which was suspended in ethanol, separated by filtration and washed with water. Recrystallization from ethanol provided methyl 1H-imidazo[4,5-c]quinolin-2-carbamate hydrate, m.p. >250° C. Analysis: Calculated for C12H10N4O2. 0.75H2O: %C, 56.4; %H, 4.5; %N, 21.9; Found: %C, 56.1; %H, 4.4; %N, 22.4.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04698348uspto-grants-1987_10