Reaktion #65727

Reaktionsgleichung

2-BOC-hydrazino-5-nitropyridine

→

2-(BOC-Hydrazino)-5-Amino-Pyridine

Ausbeute 81.6%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe reaction mixture was filtered through a filter cell plug
2. 2
   Waschenrinsed with ethanol
3. 3
   EinengenThe yellow green solution was concentrated under reduced pressure
4. 4
   Sonstigeto give a pale yellow solid
5. 5
   SonstigeThe product was recrystallized from ethanol

Vorschrift

Into a Parr hydrogenation bottle was added 2-BOC-hydrazino-5-nitropyridine (1 equivalent), 1(7% palladium on charcoal (0.3 gm Pd/gm of pyridine) and ethanol (100 ml/gm of pyridine). The reaction was hydrogenated at 50 psi H2 for 2 hours at room temperature on a Parr hydrogenator. The reaction mixture was filtered through a filter cell plug and rinsed with ethanol. The yellow green solution was concentrated under reduced pressure to give a pale yellow solid. The product was recrystallized from ethanol; yield 81.64%; m.p. 140°-142°. IR (KBr): 3360, 3200, 2980, 1650, 1635, 1580, 1490, 1390, 1360, 1300, 1260, 1160, 1020, 880, 860, 830, 750, 590, 530 cm-1.

Quelle