Reaktion #93048

Reaktionsgleichung

phenazine

nitrobenzene

dimethylsulphate

→

9-methylphenazinium methylsulphate

Ausbeute 67.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated for 7 minutes at the temperature of 100° C
2. 2
   TemperaturThen the reaction mixture is cooled with ice
3. 3
   FiltrationThe formed precipitate is filtered off
4. 4
   Waschenwashed with 30 ml of ethyl ether
5. 5
   Sonstigerecrystallized from 15 ml of ethanol

Vorschrift

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.

Quelle