反应详情

温度

70 °C

A 3.7 g portion of diethyl 4-[N-(2-cyanophenyl)carbamoyl]benzylphosphonate and 10 ml of a 40% aqueous methylamine solution were dissolved in 50 ml of THF and refluxed with heating at 70° C. for 30 hours. After completion of the reaction, the solvent was distilled off under reduced pressure. The residue was subjected to silica gel column chromatography (eluent: chloroform: methanol=100:1) and the crude crystals obtained were recrystallized from chloroform-n-hexane to provide 1.0 g of the objective compound as colorless crystals. Table 1 also shows the structure and physical property (melting point) of the compound thus obtained.

1. temperaturerefluxed
2. customAfter completion of the reaction
3. distillationthe solvent was distilled off under reduced pressure
4. customthe crude crystals obtained
5. customwere recrystallized from chloroform-n-hexane