反应详情

A solution of 4-(4-nitro-phenoxy)-piperidine (7.80 g, 35.1 mmol) and triethylamine (7.77 mL, 56.2 mmol) in DCM (100 mL) at 0° C. was treated dropwise with methanesulfonyl chloride (3.26 mL, 42.1 mmol) and stirred cold for 1 hour. The mixture was diluted with DCM, washed with 1M HCl, a saturated NaHCO3 solution, water and brine, dried over Na2SO4 and concentrated under vacuum to leave the title compound (9.10 g, 86% yield) as a yellow/orange solid. 1H NMR (300 MHz, CDCl3) δ 8.21 (d, J=9.2 Hz, 2H), 6.97 (d, J=9.2 Hz, 2H), 4.68 (m, 1H), 3.39 (m, 4H), 2.84 (s, 3H), 2.05 (m, 4H). LCMS (m/z, Method A) ES+ 301.0 [M+1]+.

1. washwashed with 1M HCl
2. dry with materiala saturated NaHCO3 solution, water and brine, dried over Na2SO4
3. concentrationconcentrated under vacuum