تفاعل #528052

ord-bb58e7b4331e41ee8af8bf942ada1173

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىWhen the exothermic reaction
  2. 2
    workup.ADDITIONare added
  3. 3
    درجة الحرارةat reflux for 25 hours
  4. 4
    درجة الحرارةcooled to 0°
  5. 5
    ترشيحfiltered
  6. 6
    غسيلWashing with 4×100 mi of ethanol/diethyl ether (1:1)
  7. 7
    أخرىdrying

الإجراء التجريبي

9.1 ml (0.13 mol) of 65% nitric acid are added dropwise in the course of 5 minutes to a yellow suspension of 20.0 g (0.13 mol) of 2-amino-4-nitrotoluene in 50 ml of absolute ethanol. When the exothermic reaction has subsided, 8.32 g (0.198 mol) of cyanamide dissolved in 8.3 ml of water are added. The brown reaction mixture is boiled at reflux for 25 hours, cooled to 0° and filtered. Washing with 4×100 mi of ethanol/diethyl ether (1:1) and drying yield 2-methyl-5-nitrophenyl-guanidine nitrate; m.p. 219°-226°.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05521184uspto-grants-1996_05