反应详情

A solution of N-{1-[(benzyloxy)carbonyl]piperidin-4-yl}-N-(tert-butoxycarbonyl)-β-alanine (4.06 g) obtained in Example 45b), WSC (1.92 g) and HOBt.NH3 (1.52 g) in DMF (40 mL) was stirred overnight at room temperature, and DMF was distilled off under reduced pressure. The residue was diluted with dichloromethane, washed with an aqueous saturated sodium bicarbonate solution and saturated saline solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (from ethyl acetate/hexane=1/1 to ethyl acetate) to obtain the title compound (3.38 g, 83%) as a white amorphous powder.

1. distillationDMF was distilled off under reduced pressure
2. additionThe residue was diluted with dichloromethane
3. washwashed with an aqueous saturated sodium bicarbonate solution and saturated saline solution
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by basic silica gel column chromatography (from ethyl acetate/hexane=1/1 to ethyl acetate)