反应详情

Tetramethyl ethenylidenebisphosphonate was synthesized via following general synthetic procedure. ##STR11## Specifically, 4.03 g (17.4 mmol) of tetramethyl methylenebisphosphonate, 2.60 g (86.7 mmol) of paraformaldehyde and 1.27 g (17.4 mmol) diethylamine were combined with the same reactants and at the same conditions as described above in Example I and refluxed for 2 hours. After the methanol was eliminated as described in Example I, 3.05 g of tetramethyl ethenylidenebisphosphonate was produced as a clear liquid with the following spectral characteristics: 1H NMR (CDCl3) 6.99 (distorted dd, 2H H2C=, J=33.9 and 37.7), (distorted dd, 12H, --OCH3, J=5.1 and 6.1); 13C NMR (CDCl3) 150.2 (s, H2C=), 130.2 (t, PCP, J=168), 53.2 (s, --OCH3); 31P NMR (CDCl3) +15.5. Anal. Calcd for C5H14O6P2 : C, 29.52; H, 5.78; P, 25.38. Found: C, 29.26 ; H, 6.01; P, 25.19.

1. customTetramethyl ethenylidenebisphosphonate was synthesized
2. temperaturerefluxed for 2 hours