Reaktion #54148

Reaktionsgleichung

2-chloro-5-nitropyridine

hydrazine

→

2-Hydrazino-5-nitropyridine

Lösungsmittel

methanol

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added
2. 2
   Sonstigea greenish-yellow precipitate separated
3. 3
   Temperaturat reflux for 30 minutes
4. 4
   FiltrationThe greenish solid was filtered off
5. 5
   Waschenwashed with cold methanol
6. 6
   Waschenwashed
7. 7
   Sonstigevacuum dried

Vorschrift

To a slurry of 47.6 g (0.3 mol) of 2-chloro-5-nitropyridine in a mixture of 400 ml methanol and 60 ml water and cooled to 10° C. was added with cooling below 30° 86 g hydrazine (95 percent) over about 10 minutes. The solids first went into solution, then a greenish-yellow precipitate separated. The mixture was stirred at reflux for 30 minutes. The greenish solid was filtered off and washed with cold methanol. The solid was slurried in 200 ml of cold water, washed and vacuum dried. The yield was 40.1 g (87 percent).

Quelle