反应详情

温度

120 °C

2d (0.78 g, 1.76 mmol) and 43b (0.66 g, 3.39 mmol) were combined with diisopropylethylamine (0.91 mL, 5.5 mmol) in DMSO (8 mL) and heated to 120° C. overnight. The mixture was cooled to room temperature and poured into 20 mL of ethyl acetate, washed with water (20 mL) and brine (3×20 mL), dried and concentrated. The residue was purified by flash chromatography (eluent: 50 to 90% of EtOAc+0.1% triethylamine in hexane) to afford 4-[1-(2,5-difluoro-4-methanesulfinyl-phenyl)-piperidin-4-ylideneaminooxy]-piperidine-1-carboxylic acid isopropyl ester 43-1. This material was recrystallized from toluene and hexane to afford 43-1 as a white powder: HPLC, LC-MS 458.1 (MH), tR=6.98 (Method 2). EC50: 58 nM.

1. temperatureThe mixture was cooled to room temperature
2. washwashed with water (20 mL) and brine (3×20 mL)
3. customdried
4. concentrationconcentrated
5. customThe residue was purified by flash chromatography (eluent: 50 to 90% of EtOAc+0.1% triethylamine in hexane)