反应详情

The 5-(tert-butoxycarbonylamino)pentanoic acid (424 mg, 1.95 mmol) was introduced into a microwave vial charged with DMAP (238 mg, 1.95 mmol) and Intermediate 20A (400 mg, 1.95 mmol). The reactants were dissolved in DMF (5 mL) and the DIC (0.304 mL, 1.95 mmol) was added. The reaction mixture was stirred at rt overnight. The reaction mixture was diluted with 3 mL of pyridine. The vial was capped and the reaction was heated in the microwave at 145° C. for 20 min. The reaction mixture was allowed to cool to rt. The reaction mixture was diluted with EtOAc and washed with water and brine. The organic portion was concentrated under reduced pressure and purified by silica gel chromatography with EtOAc/Hexane to give Intermediate 20B as a white solid (230 mg, 0.595 mmol, 30.5% yield). HPLC/MS (Method D) RT=2.40 min [M+H]+ 385.9.

1. customThe vial was capped
2. temperaturethe reaction was heated in the microwave at 145° C. for 20 min
3. temperatureto cool to rt
4. washwashed with water and brine
5. concentrationThe organic portion was concentrated under reduced pressure
6. custompurified by silica gel chromatography with EtOAc/Hexane