反应详情

To a solution of compound 47a (144 mg, 0.240 mmol) in DCM (1 mL) was added TFA (0.8 mL). The resulting mixture was stirred at rt for 1 h and concentrated under reduced pressure. The residue obtained was dried under reduced pressure overnight, suspended in 20 mL of diethyl ether, sonicated for 5 min and concentrated. The solid obtained was dried under reduced pressure for 4 h to obtain a residue which was dissolved in 1:1 MeOH/DCM solution (5 mL) and filtered through a sodium bicarbonate cartridge. The filtrate was concentrated under reduced pressure and the resulting residue was triturated in ether to give compound 47b. Mass Spectrum (LCMS, ESI pos.) Calcd. for C29H30N8O2: 523.2 (M+H). Found 523.3.

1. concentrationconcentrated under reduced pressure
2. customThe residue obtained
3. customwas dried under reduced pressure overnight
4. customsonicated for 5 min
5. concentrationconcentrated
6. customThe solid obtained
7. customwas dried under reduced pressure for 4 h
8. customto obtain a residue which
9. filtrationfiltered through a sodium bicarbonate cartridge
10. concentrationThe filtrate was concentrated under reduced pressure
11. customthe resulting residue was triturated in ether