反应详情

4-Azidobenzoic acid (858 mg, 5.15 mmol), HOBt (704 mg, 5.15 mmol, 1.0 eq.) and N-(2-aminoethyl)piperidine (0.788 ml, 5.41 mmol, 1.05 eq.) were dissolved in acetonitrile (6 ml) and DMF (6 ml), WSC (1.21 g, 6.19 mmol, 1.2 eq.) was added, and the mixture was stirred at room temperature for 3 hr. The reaction mixture was concentrated, dissolved in ethyl acetate (50 ml) and washed with 5% aqueous sodium carbonate solution and saturated brine. The aqueous layers were each extracted with ethyl acetate (30 ml). The organic layers were combined, dried over anhydrous sodium sulfate and concentrated at 30° C. or below to give the title compound as a pale-yellow oil.

1. concentrationThe reaction mixture was concentrated
2. dissolutiondissolved in ethyl acetate (50 ml)
3. washwashed with 5% aqueous sodium carbonate solution and saturated brine
4. extractioneach extracted with ethyl acetate (30 ml)
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated at 30° C. or below