반응 #2072

반응 방정식

ammonium formate

tetraethyl 3-nitrooctane-1,1-bisphosphonate

ammonium formate

→

title compound

수율 95.0%

tetraethyl 3-aminooctane-1,1-bisphosphonate

수율 95.0%

용매

methanol

반응 조건

후처리

1. 1
   여과the reaction mixture was filtered
2. 2
   세척rinsing the residue with methanol
3. 3
   농축concentrated
4. 4
   추출extracted with dichloromethane (4×15 mL)
5. 5
   건조dried (Na2SO4)
6. 6
   농축concentrated

실험 절차

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.

출처