反应详情

The product from Example Z (1.15 g, 4.50 mmol) was dissolved in 50 mL of THF at room temperature with stirring. To the solution were added O-(7-azabenzotriazol-1-y-)-1,1,3,3-tetramethyluronium hexafluorophosphate (HATU, 3.11 g, 8.18 mmol), 1-hydroxy-7-azabenzotriazole (HOAt, 1.11 g, 8.18 mmol), N,N-diisopropylethylamine (DIEA, 2.84 mL, 16.36 mmol) followed by the product from Example M (1.34 g, 4.09 mmol) in 50 mL of THF. After 3 hours, the solution was concentrated under reduced pressure, partitioned between ethyl ether and water (100 mL each), and separated. The organic layer was washed with 5% sodium bicarbonate (2×50 mL), brine (2×50 mL), dried with magnesium sulfate, filtered, and concentrated under reduced pressure to a solid. The solid was purified by silica gel chromatography with ethyl acetate. Appropriate fractions were combined and concentrated under reduced pressure to a solid (2.17 g).

1. concentrationthe solution was concentrated under reduced pressure
2. custompartitioned between ethyl ether and water (100 mL each)
3. customseparated
4. washThe organic layer was washed with 5% sodium bicarbonate (2×50 mL), brine (2×50 mL)
5. dry with materialdried with magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure to a solid
8. customThe solid was purified by silica gel chromatography with ethyl acetate
9. concentrationconcentrated under reduced pressure to a solid (2.17 g)