反应详情

Compound 12 (0.71 g, 1.4 mmol) and compound 25 (0.57 g, 1.2 mmol) were dissolved in 10 ml DMF and HBTU (0.8 g, 2.1 mmol) was added as a solid followed by DIEA (0.52 ml, 3 mmol). The reaction mixture was stirred at room temperature for 3 days, diluted with EtOAc and the organic phase washed with saturated NaHCO3. The aqueous layer was back extracted with EtOAc twice and the combined organic layers dried over MgSO4, filtered and concentrated to an oil. This oil was purified by flash silica chromatography (2 to 5% MeOH/EtOAc) to give an orange oil (0.50 g, 0.52 mmol, 44%, compound 27).

1. washthe organic phase washed with saturated NaHCO3
2. extractionThe aqueous layer was back extracted with EtOAc twice
3. dry with materialthe combined organic layers dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated to an oil
6. customThis oil was purified by flash silica chromatography (2 to 5% MeOH/EtOAc)