反应详情

温度

40 °C

To a mixture of 2-(Dipropylamino)isonicotinic acid hydrochloride (0.2 g) in methylene chloride (15 mL) was added triethylamine (0.195 g), HOBT (0.105 g), and HATU (0.293 g). The mixture was stirred at 39° C. for 10 minutes at which time (2R,3S)-3-amino-4-(3,5-difluorophenyl)-1-[(3-ethylbenzyl)amino]butan-2-ol (0.285 g) was added. The mixture was stirred at 40° C. for 4 h then poured into methylene chloride (50 mL), washed with water then brine, dried over anhydrous magnesium sulfate and concentrated under vacuum. Column chromatography on silica gel (100 mL) using 5% methanol in methylene chloride as eluent and conversion to the hydrochloride salt gave 0.105 g of the title compound: MS (ESI+) for C31H40F2N4O2 m/z 539.3 (M+H)+.

1. additionwas added
2. washwashed with water
3. dry with materialbrine, dried over anhydrous magnesium sulfate
4. concentrationconcentrated under vacuum