反应详情

A mixture of 1-benzyl-4-[N-methyl-N-(3-amino-2-pyridinyl)amino]piperidine (EXAMPLE 122, 825 mg), 1-bromo-1-ethoxycyclopropane (919 mg) and triethylamine (0.78 ml) in dry tetrahydrofuran (1.4 ml) under nitrogen is refluxed for 48 hrs, cooled to 20°-25°, diluted with methylene chloride (30 ml), washed with saline (10 ml), dried over sodium sulfate and concentrated under reduced pressure to give the crude product. The residue is chromatographed (silica gel, 70-230 mesh, 140 g; eluting with a gradient of methanol/methylene chloride (1/99-5/95)) to give the title compound, NMR (CDCl3) 7.80, 7.41, 7.25, 6.93, 5.62, 3.51, 3.48, 3.03, 2.87, 2.60, 1.98, 1.71, 1.64, 1.13 and 0.85δ.

1. temperatureis refluxed for 48 hrs
2. temperaturecooled to 20°-25°
3. washwashed with saline (10 ml)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customto give the crude product
7. customThe residue is chromatographed (silica gel, 70-230 mesh, 140 g
8. washeluting with a gradient of methanol/methylene chloride (1/99-5/95))