反应详情

To a stirred solution of 3-[1-(4-pyridinylmethyl)-2-pyrrolidinyl]phenol (0.60 g) in dry tetrahydrofuran (16 ml) was added milled potassium carbonate (0.36 g), followed by methyl isocyanate (0.15 ml), dropwise, at ambient temperature, under nitrogen, with stirring. The mixture was stirred for 17 hrs and filtered through a pad of celite. The filter cake was washed with ethyl acetate, and the filtrate was concentrated. The residue was purified by flash column chromatography (silica gel, ether). The appropriate fractions were collected and concentrated to afford 0.63 g (86%) of product. Trituration of the residue with petroleum ether gave the analytical sample, mp 92°-105° C.

1. stirringThe mixture was stirred for 17 hrs
2. filtrationfiltered through a pad of celite
3. washThe filter cake was washed with ethyl acetate
4. concentrationthe filtrate was concentrated
5. customThe residue was purified by flash column chromatography (silica gel, ether)
6. customThe appropriate fractions were collected
7. concentrationconcentrated