Reaktion #2250806

Reaktionsgleichung

hydrochloric acid

2,6-dinitro-N-(1-ethylpropyl)-3,4-dimethylaniline

2,6-dinitro-N-nitroso-N-(1-ethylpropyl)-3,4-dimethylaniline

sulfamic acid

→

N-(1-Ethylpropyl)-3,4-dimethylaniline

Lösungsmittel

ethylene dichloride

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe aqueous phase was separated
2. 2
   ExtraktionThe aqueous phase was extracted with 500 ml
3. 3
   WaschenThe combined organic phase was washed with 3-liters of water
4. 4
   Sonstigethe aqueous phase separated
5. 5
   Sonstigethe ethylene dichloride was removed under vacuum at 68° C.
6. 6
   Sonstigeto recover 1915 g
7. 7
   workup.ADDITIONof product containing 1820 g

Vorschrift

To a crude nitration solution comprising 1550 g. of 2,6-dinitro-N-(1-ethylpropyl)-3,4-dimethylaniline and 340 g. of 2,6-dinitro-N-nitroso-N-(1-ethylpropyl)-3,4-dimethylaniline in 3700 mls. of ethylene dichloride was added 212 g. of sulfamic acid and 2850 mls. of 37.7% hydrochloric acid. The mixture was refluxed at 80° C. for six hours, 2-liters of water was added thereto and the aqueous phase was separated. The aqueous phase was extracted with 500 ml. of ethylene dichloride and the organic phases were combined. The combined organic phase was washed with 3-liters of water, the aqueous phase separated and the ethylene dichloride was removed under vacuum at 68° C. to recover 1915 g. of product containing 1820 g. of 2,6-dinitro-N-(1-ethylpropyl)-3,4-dimethylaniline and less than 0.1% of 2,6-dinitro-N-nitroso-N-(1-ethylpropyl)-3,4-dimethylaniline.

Quelle