Reaktion #215032

Reaktionsgleichung

7-Chloro-5-(2-fluorophenyl)-1,3-dihydro-2-nitromethylene-2H-1,4-benzodiazepine-4-oxide

sodium nitrite

sodium nitrite

→

7-Chloro-5-(2-fluorophenyl)-N-hydroxy-α-nitro-3H-1,4 -benzodiazepine-2-methanimine 4-oxide

Lösungsmittel

acetic acid

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISSOLUTIONwas dissolved
2. 2
   Sonstigereached 70° C.
3. 3
   Temperaturwhile cooling
4. 4
   workup.ADDITIONthe addition
5. 5
   Extraktionextracted with methylene chloride
6. 6
   WaschenThe extracts were washed with water
7. 7
   Trocknendried over sodium sulfate
8. 8
   Sonstigeevaporated
9. 9
   SonstigeCrystallization of the residue from ethyl acetate yielded yellow crystals

Vorschrift

7-Chloro-5-(2-fluorophenyl)-1,3-dihydro-2-nitromethylene-2H-1,4-benzodiazepine-4-oxide* 7 g (0.02 mole), was dissolved by heating in 250 ml of glacial acetic acid. The solution was cooled with tap water and when the temperature reached 70° C. the addition of 1.9 g (0.0275 mole) of sodium nitrite was started. The sodium nitrite was added over a period of 10 min while cooling was continued. Following the addition, the mixture was stirred for 11/2 hr at room temperature, diluted with water and extracted with methylene chloride. The extracts were washed with water, dried over sodium sulfate and evaporated. Crystallization of the residue from ethyl acetate yielded yellow crystals.

Quelle