反应详情

To 30 mg (0.055 mmol) of amine 7-2 in CH2Cl2 was added 10 mg (0.097 mmol) of N,N-dimethylglycine and 15 mg (0.078 mmol) of EDCI. After stirring overnight at room temperature, the mixture was partitioned between CH2Cl2 and saturated NaHCO3, the layers were separated, the organic phase was washed with water, dried over Na2SO4, and concentrated by rotary evaporation. The residue was dissolved in dry CH3CN and ˜500 μL of 3HF-TEA was added and the mixture was stirred overnight at room temperature. The reaction was partitioned between EtOAc and saturated NaHCO3, the layers were separated, the organic phase was washed with brine, dried over Na2SO4, and concentrated by rotary evaporation. The residue was purified by reverse phase HPLC to provide 7-3 as a white solid. Data for 7-3: HRMS (ES) calc'd M+H for C28H34F2N4O3: 513.2672. Found: 513.2673.

1. customthe mixture was partitioned between CH2Cl2 and saturated NaHCO3
2. customthe layers were separated
3. washthe organic phase was washed with water
4. dry with materialdried over Na2SO4
5. concentrationconcentrated by rotary evaporation
6. dissolutionThe residue was dissolved in dry CH3CN
7. addition˜500 μL of 3HF-TEA was added
8. stirringthe mixture was stirred overnight at room temperature
9. customThe reaction was partitioned between EtOAc and saturated NaHCO3
10. customthe layers were separated
11. washthe organic phase was washed with brine
12. dry with materialdried over Na2SO4
13. concentrationconcentrated by rotary evaporation
14. customThe residue was purified by reverse phase HPLC