تفاعل #93048

ord-4131871b38af4fd5ae319ab0057b9ff1

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةheated for 7 minutes at the temperature of 100° C
  2. 2
    درجة الحرارةThen the reaction mixture is cooled with ice
  3. 3
    ترشيحThe formed precipitate is filtered off
  4. 4
    غسيلwashed with 30 ml of ethyl ether
  5. 5
    أخرىrecrystallized from 15 ml of ethanol

الإجراء التجريبي

1.76 g (0.011 mol) of phenazine and 33.5 ml of dry nitrobenzene are heated to boiling, cooled to 100° C., added with 12.2 g (0.011 mol) of freshly distilled dimethylsulphate and heated for 7 minutes at the temperature of 100° C. Then the reaction mixture is cooled with ice and allowed to stand for 48 hours at the temperature of 4° C. in a refrigerator. The formed precipitate is filtered off, washed with 30 ml of ethyl ether and recrystallized from 15 ml of ethanol. 2.0 g of 9-methylphenazinium methylsulphate (67%) are thus obtained in the form of yellowish crystals melting at 155°-157° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04610767uspto-grants-1986_09