反应详情

This compound was prepared from N-methyl-N-chloroethylamine.HCl via N-methyl-N-(2-chloroethyl)phosphoramidic dichloride, as described for 16a (14 mmol scale). The crude residue was purified by chromatography (1:4 EtOAc:hexanes) to give 16b as an oil (2.72 g, 61%): Rf 0.75 (1:1 EtOAc:hexanes); 1H NMR (CDCl3) 4.22(m, 4H), 3.60(m, 3H), 3.42(m, 2H), 2.80(d, 3H, J=12.85 Hz), 1.99(dt, 2H, J=6.11 Hz), 1.36(d, 6H, J=15.82 Hz)ppm; -P NMR (CDCl3) -7.69, -7.92 ppm (1:1 ratio of diastereomers).

1. customThe crude residue was purified by chromatography (1:4 EtOAc:hexanes)