Réaction #1069708

Équation de réaction

2-(1-Piperazinyl)-3-nitropyridine

hydrochloric acid

→

3-amino-2-(1-piperazinyl)pyridine

Solvants

ethanol

Conditions de réaction

Traitement

1. 1
   FiltrationThe mixture is filtered through celite
2. 2
   Lavagewashed with ethanol, chloroform, ethanol and water
3. 3
   AutreThe organic solvents are removed with head and reduced pressure
4. 4
   AutreThe remaining material is partitioned between methylene chloride (3×250 ml) and sodium bicarbonate
5. 5
   Séchagedried over potassium carbonate
6. 6
   Filtrationfiltered
7. 7
   Concentrationconcentrated under reduced pressure
8. 8
   Autreto give an oil which

Mode opératoire

2-(1-Piperazinyl)-3-nitropyridine (24.50 g), ethanol (445 ml) and hydrochloric acid (1.2N, 44 ml) are combined and hydrogenated overnight at 40 psi initial pressure in a Parr Bomb, refilling when necessary. The mixture is filtered through celite, washed with ethanol, chloroform, ethanol and water. The organic solvents are removed with head and reduced pressure. The remaining material is partitioned between methylene chloride (3×250 ml) and sodium bicarbonate. The organic layers are combined, dried over potassium carbonate, filtered and concentrated under reduced pressure to give an oil which slowly solidified upon standing to give 3-amino-2-(1-piperazinyl)pyridine.

Source