反应详情

A mixture of diethyl cyanomethylphosphonate (17.7 g; 0.1 moles) in ethanol (70 ml) and aqueous HCl (40 ml of 10% HCl) over 10% Pd/C (1 g) is stirred in a pressure vessel at 60 psi. When the calculated amount of H2 had been absorbed (about 26 hours), the catalyst is filtered off over Celite, washed with ethanol, and the filtrate is neutralized with NaHCO3 and evaporated to dryness under vacuum. The residue is extracted with absolute ethanol (2×50 ml) and the clear extract is distilled at about 110° C. and 0.18 mbar to give a colorless liquid (11.4 g; yield 63%).

1. customWhen the calculated amount of H2 had been absorbed (about 26 hours)
2. filtrationthe catalyst is filtered off over Celite
3. washwashed with ethanol
4. customevaporated to dryness under vacuum
5. extractionThe residue is extracted with absolute ethanol (2×50 ml)
6. extractionthe clear extract
7. distillationis distilled at about 110° C.
8. custom0.18 mbar to give a colorless liquid (11.4 g; yield 63%)