反应详情

温度

100 °C

Add 1 mL of conc. hydrochloric acid into a solution of 4-[6-(2-chloro-4-fluoro-benzoylamino)-pyridin-2-yloxy]-cis-2-methyl-piperidine-1-carboxylic acid tert-butyl ester isomer 2 (preparation 109, 0.678 g) in 1,4-dioxane 20 mL and heat at 100° C. After 40 min., partition between ethyl acetate and saturated aqueous NaCl, dry over anhydrous sodium sulfate, evaporate and purify on a silica gel column eluting with dichloromethane-2M NH3 in methanol, gradient to give the title compound (0.53 g). Mass spectrum (electric spray) m/z=364 (M+1); 1H NMR (CDCl3): 8.53 (br s, 1H), 7.84 (br d, 1H), 7.73 (dd, 1H), 7.63 (dd, 1H), 7.21 (dd, 1H), 7.10 (ddd, 1H), 6.49 (dd, 1H), 4.93 (m, 1H), 3.14 (m, 1H), 2.78 (m, 2H), 2.12 (m, 2H), 1.75 (br, 1H), 1.48 (m, 1H), 1.19 (m, 1H), 1.12 (d, 3H).

1. custompartition between ethyl acetate and saturated aqueous NaCl
2. dry with materialdry over anhydrous sodium sulfate
3. customevaporate
4. custompurify on a silica gel column
5. washeluting with dichloromethane-2M NH3 in methanol, gradient