Reaktion #2253236

Reaktionsgleichung

N-cyclohexyl-4-(1H-imidazol-1-ylmethyl)-2-nitrobenzenamine

sodium dithionite

ethanol

→

N1 -cyclohexyl-4-(1H-imidazol-1-ylmethyl)-1,2-benzenediamine

Ausbeute 98.0%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeUpon complete reaction
2. 2
   Sonstigethe ethanol layer was evaporated
3. 3
   workup.ADDITIONThe aqueous layer was diluted with a potassium carbonate solution
4. 4
   ExtraktionThe whole was extracted twice
5. 5
   workup.ADDITIONfirst with dichloromethane and then with a mixture of trichloromethane and methanol (90:10 by volume)
6. 6
   SonstigeThe combined extracts were dried
7. 7
   Filtrationfiltered
8. 8
   Sonstigeevaporated
9. 9
   Sonstigethe solvent was evaporated again

Vorschrift

A mixture of 7.9 parts of N-cyclohexyl-4-(1H-imidazol-1-ylmethyl)-2-nitrobenzenamine, 22.9 parts of sodium dithionite, 288 parts of ethanol and 240 parts of water was stirred at room temperature. Upon complete reaction, the ethanol layer was evaporated. The aqueous layer was diluted with a potassium carbonate solution. The whole was extracted twice: first with dichloromethane and then with a mixture of trichloromethane and methanol (90:10 by volume). The combined extracts were dried, filtered and evaporated. The residue was taken up in methylbenzene and the solvent was evaporated again, yielding 7 parts (98.0%) of N1 -cyclohexyl-4-(1H-imidazol-1-ylmethyl)-1,2-benzenediamine as a residue (int. 186).

Quelle