反应详情

Intermediate 41 (0.22 g, 0.37 mmol) was dissolved in acetone (50 mL) to give a colorless solution. The reaction mixture was diluted with water (20 mL) and TFA (2 mL), heated to reflux for 2 h, then cooled and concentrated. The precipitated product was isolated by suction filtration. A small amount of toluene (5 mL) was added to the wet solid, the mixture was concentrated to remove water azeotropically, and dried in vacuum to afford intermediate 42 (0.21 g, 103% yield, presumably as tri-fluoroacetate salt). MS (m/z): 553.2 (M+H).

1. customto give a colorless solution
2. temperatureheated
3. temperatureto reflux for 2 h
4. temperaturecooled
5. concentrationconcentrated
6. customThe precipitated product was isolated by suction filtration
7. concentrationthe mixture was concentrated
8. customto remove water azeotropically
9. customdried in vacuum