Reaktion #2170811

Reaktionsgleichung

sodium bicarbonate

N-(1-Ethylpropyl)-2,6-dinitro-3,4-xylidine

ethanol

sodium sulfide nonahydrate

→

N4 -(1-Ethylpropyl)-3-nitro-o-xylene-4,5-diamine

Lösungsmittel

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted 3 times with 1 liter portion of ether
2. 2
   Trocknendried over magnesium sulfate
3. 3
   SonstigeRemoval of the drying agent and solvent
4. 4
   Sonstigeleaves a dark solid which
5. 5
   Sonstigeis recrystallized 3 times from hexane

Vorschrift

N-(1-Ethylpropyl)-2,6-dinitro-3,4-xylidine (100 g.) is dissolved in 2500 ml. of ethanol and a solution of sodium sulfide nonahydrate (240 g.) and sodium bicarbonate (84 g.) in 500 ml. of water is added at 25°-42° C. The mixture is heated to 65° C. and held at 60°-65° C. for 3 hours. The mixture is then poured into water and extracted 3 times with 1 liter portion of ether. The ether extracts are combined and dried over magnesium sulfate. Removal of the drying agent and solvent leaves a dark solid which is recrystallized 3 times from hexane and then 3 times from hexane-ethanol. The product (35.0 g.), an orange solid, has m.p. 80°-82° C. Analysis Calcd. for C13H21N3O2 : C, 62.12; H, 8.41; N, 16.71. Found: C, 62.41; H, 8.33; N, 16.47.

Quelle