反应详情

A solution of acid 5b (93.0 mg, 0.348 mmol), amine hydrochloride 6b (80.0 mg, 0.418 mmol) and HATU (139 mg, 0.365 mmol) in dry DMF (2 mL) was cooled to 0° C. and DIEA (0.182 mL, 1.04 mmol) was added dropwise over 5 minutes. The mixture was allowed to reach rt over 2 h and stirred at rt for 20 h. The mixture was poured into deionized H2O (10mL) and extracted with EtOAc (3×). The combined extracts were washed sequentially with 1M Na2CO3, deionized H2O, 0.5 M HCl (2×) and brine. The EtOAc solution was dried over MgSO4 and filtered through a SiO2 plug capped with a layer of MgSO4. The solution was concentrated to give the title compound 7b as a bronze glass which was scraped to a tan solid; 81 mg, 58%, MS m/z 403.1 (ESI−, M−1).

1. extractionextracted with EtOAc (3×)
2. washThe combined extracts were washed sequentially with 1M Na2CO3
3. dry with materialThe EtOAc solution was dried over MgSO4
4. filtrationfiltered through a SiO2 plug
5. customcapped with a layer of MgSO4
6. concentrationThe solution was concentrated