反应详情

1-(1-(4-fluorobenzyl)-1H-indole-2-carbonyl)piperidine-4-carboxylic acid (100 mg, 0.263 mmol), 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide (76 mg, 0.394 mmol), and 1-Hydroxybenzotriazole (53 mg, 0.394 mmol) were dissolved in 3.0 mL of DCM. The reaction was allowed to stir for 10 minutes before N,N-Diisopropylethylamine (68.9 μL, 0.504 mmol) and (R)-1-phenylethanamine (64 μL, 0.504 mmol) were added. The reaction was allowed to stir for 48 hours. The reaction was diluted with water and ethyl acetate. The layers were separated and the organic layer was washed with another aliquot of water. The ethyl acetate layer was washed with saturated citric acid, saturated sodium bicarbonate, and saturated sodium chloride. The organic layer was dried over magnesium sulfate, filtered and concentrated. The crude material was triturated in methanol, filtered and dried under vacuum to obtain pure product as a white solid. Yield: 32.9 mg (White solid)

1. additionwere added
2. customThe layers were separated
3. washthe organic layer was washed with another aliquot of water
4. washThe ethyl acetate layer was washed with saturated citric acid, saturated sodium bicarbonate, and saturated sodium chloride
5. dry with materialThe organic layer was dried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude material was triturated in methanol
9. filtrationfiltered
10. customdried under vacuum
11. customto obtain pure product as a white solid