反应详情

In a 2-5 microwave vial, placed in a dry-ice acetone bath, was added THF (2 mL) and CH3CN (2 mL) to a mixture of Intermediate 25 (156.19 mg; 0.50 mmol), Intermediate 34 (114.32 mg; 0.50 mmol) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (115.02 mg; 0.60 mmol). The reaction mixture was allowed to warm to RT for half a hour then DIEA (204.07 μL; 1.20 mmol) was added and the mixture was heated by microwave irradiation at 150° C. for 30 min. The reaction mixture was filtered through a SPE NH2 column (2 g) and rinsed with ACN. The filtrate was passed through a SPE SCX column (2 g) and rinsed with ACN. After evaporation of the solvents, the crude product was purified by flash chromatography (c-hex/EtOAc: 9.5/0.5), affording the title compound. LC/MS (Method B): 503.4 (M−H)−, 505.3 (M+H)+. HPLC (Method A) Rt 5.64 min (Purity: 100.0%).

1. customIn a 2-5 microwave vial, placed in a dry-ice acetone bath
2. temperaturethe mixture was heated by microwave irradiation at 150° C. for 30 min
3. filtrationThe reaction mixture was filtered through a SPE NH2 column (2 g)
4. washrinsed with ACN
5. washrinsed with ACN
6. customAfter evaporation of the solvents
7. customthe crude product was purified by flash chromatography (c-hex/EtOAc: 9.5/0.5)