Reaktion #2072

Reaktionsgleichung

ammonium formate

tetraethyl 3-nitrooctane-1,1-bisphosphonate

ammonium formate

→

title compound

Ausbeute 95.0%

tetraethyl 3-aminooctane-1,1-bisphosphonate

Ausbeute 95.0%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationthe reaction mixture was filtered
2. 2
   Waschenrinsing the residue with methanol
3. 3
   Einengenconcentrated
4. 4
   Extraktionextracted with dichloromethane (4×15 mL)
5. 5
   Trocknendried (Na2SO4)
6. 6
   Einengenconcentrated

Vorschrift

To a stirred solution of tetraethyl 3-nitrooctane-1,1-bisphosphonate (0.70 g, 1.62 mmol) in methanol (4 mL) was added ammonium formate (0.45 g, 6.9 mmol) and 10% palladium on carbon (0.070 g). After 24 hours, more 10% palladium on carbon (0.035 g) and ammonium formate (0.45 g, 6.9 mmol) were added. After stirring for a total of 4 days, the reaction mixture was filtered, rinsing the residue with methanol, and concentrated. The residue was taken up in brine (5 mL) and extracted with dichloromethane (4×15 mL), dried (Na2SO4) and concentrated to give the title compound (0.60 g, 95%) as an oil.

Quelle