反应详情

温度

35 °C

Method E—Step a To a vial with 1-[4-Chloro-3-(5-methyl-1H-benzoimidazol-2-yl)-phenyl]-pyrrolidine-3-carboxylic acid (obtained as described in general method 5, step b) (0.09 g, 0.25 mmol), HATU (0.10 g, 0.26 mmol), TEA (0.07 mL, 0.53 mmol) and morpholine (0.03 mL, 0.33 mmol) dichloromethane (2 mL) was added and the reaction mixture was heated at 35° C. overnight. Reaction was cooled to room temperature, saturated NaHCO3 solution (2 mL) was added with stirring, the organic layer recovered by filtration through phase separator, and the solvent removed under reduced pressure. The crude was purified by NH2 column (eluent: dichloromethane:MeOH from 10:0 to 5:5), and SCX to obtain 0.05 g of the title compound (46%).

1. customReaction
2. temperaturewas cooled to room temperature
3. filtrationthe organic layer recovered by filtration through phase separator
4. customthe solvent removed under reduced pressure
5. customThe crude was purified by NH2 column (eluent: dichloromethane:MeOH from 10:0 to 5:5), and SCX