反应详情

NCS (370 mg, 2.83 mmol) was added to a solution of N-(1-(4-(pyridin-2-yl)pyrimidin-2-yl)piperidin-4-yl)methanesulfonamide (180 mg, 2.36 mmol) in AcOH (10 mL) at 60° C. and the reaction solution was stirred for 2 h. LC-MS indicated the reaction was almost complete. The reaction solution was concentrated and purified by chromatography, eluted with CH2Cl2:MeOH (6:1) to give crude product, which was further purified by Prep-HPLC to give title compound (251 mg, 29%) as a yellow solid. 1H NMR (400 MHz, CDCl3): δ 8.68-8.70 (d, 1H), 8.29 (s, 1H), 7.75-7.79 (m, 1H), 7.70-7.72 (d, 1H), 7.31-7.34 (t, 1H), 4.60-4.63 (d, 2H), 4.18-4.20 (d, 1H), 3.53-3.57 (t, 1H), 2.94 (s, 3H), 1.99-2.02 (d, 1H), 1.39-1.49 (m, 1H); m/z for C15H18ClN5O2S 390.1 (M+Na)+.

1. concentrationThe reaction solution was concentrated
2. custompurified by chromatography
3. washeluted with CH2Cl2:MeOH (6:1)
4. customto give crude product, which
5. customwas further purified by Prep-HPLC