反应详情

A solution of N-(1-(6-chloro-2,3-dihydrobenzo[b][1,4]dioxin-8-yl)ethyl)-2-(methylsulfonyl)-5-(piperazin-1-yl)benzenamine (50.0 mg, 0.11 mmol) in anhydrous dichloromethane (1 mL) was cooled to 0° C. and HCl (0.12 mL of a 1 M solution in diethyl ether, 0.12 mmol) was added. The mixture was allowed to stir for 30 min. The solvent was removed by rotary evaporation, more diethyl ether was added to precipitate the salt. After removal of solvent by rotary evaporation the desired product was collected (53 mg, 99%). 1H NMR (400 MHz, CD3OD): δ 7.55 (d, 1H), 6.87 (d, 1H), 6.76 (d, 1H), 6.40 (dd, 1H), 6.02 (d, 1H), 4.84 (m, 1H), 4.33 (m, 2H), 4.27 (m, 2H), 4.43 (m, 4H), 3.30 (m, 4H), 3.07 (s, 3H), 1.54 (d, 3H); MS (ESI) m/z: 452.3 (M++1).

1. customThe solvent was removed by rotary evaporation, more diethyl ether
2. additionwas added
3. customto precipitate the salt
4. customAfter removal of solvent
5. customby rotary evaporation the desired product
6. customwas collected (53 mg, 99%)