Reaktion #354681

Reaktionsgleichung

2,6-di(methylamino)-3,5-dinitropyridine

methanesulfonic acid

hydrogen

hydrogen

→

3,5-diamino-2,6-di(methylamino)pyridine

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONthe mixture was treated with anhydrous silica gel (25 g)
2. 2
   Filtrationfiltered free of catalyst
3. 3
   Sonstigedrying agent under a nitrogen atmosphere
4. 4
   Sonstigemethanol removed under vacuum

Vorschrift

A 250 ml Parr bottle was charged with 2,6-di(methylamino)-3,5-dinitropyridine (20.0 g, 0.088 mole), 30 ml methanesulfonic acid, 200 ml methanol and 1.0 g 5% Pd/charcoal catalyst. The mixture was subjected to hydrogenation at ambient temperature with an initial hydrogen pressure of 65 psig. When no further uptake of hydrogen was observed, the mixture was treated with anhydrous silica gel (25 g), filtered free of catalyst and drying agent under a nitrogen atmosphere, and methanol removed under vacuum. The trimethanesulfonate salt of 3,5-diamino-2,6-di(methylamino)pyridine was obtained under nitrogen by addition of cold i-butanol-benzene to the concentrate, followed by vacuum drying (40°-50°C) over P2O5.

Quelle