反应详情

A mixture of diethyl[3-(N-phthalimido)]propylphosphonate (ex. 5) (3.72 g; 11.4 mmoles), absolute ethanol (46 ml) and hydrazine hydrate (0.78 ml of 98% purity; 15.7 mmoles) is stirred at reflux for 35 min. The mixture is filtered and the solvent is distilled under vacuo. The resulting oil is dissolved in CHCl3 (10 ml) and is filtered again. Solvent removal in vacuo gives a colorless liquid (0.7 g; yield 30%). According to example 4, diethyl 3-aminopropylphosphonate (6) is also obtained from diethyl 2-cyanoethylphosphonate in an analogous fashion followed by vacuum distillation at about 115° C. and 0.18 mbar (yield 80%).

1. temperatureat reflux for 35 min
2. filtrationThe mixture is filtered
3. distillationthe solvent is distilled under vacuo
4. dissolutionThe resulting oil is dissolved in CHCl3 (10 ml)
5. filtrationis filtered again
6. customSolvent removal in vacuo
7. customgives a colorless liquid (0.7 g; yield 30%)