反应详情

To (S)-(9H-fluoren-9-yl)methyl (2-((di-tert-butoxyphosphoryl)oxy)-1-(3-fluoro-5-iodophenyl)ethyl)carbamate (6450 mg, 9.27 mmol) was added DMF (Volume: 90 mL) followed by piperidine (25 mL, 253 mmol) and stirred at room temperature for 30 minutes, followed by LCMS. To the crude reaction mixture was added 750 ml of ethyl acetate, washed with saturated sodium bicarbonate (2×), water (5×), saturated salt solution, dried sodium sulfate, and filtered. The solvent was concentrated off to constant mass under high vacuum to give the desire crude product which includes FMOC piperidine impurity, used as is. LCMS (m/z): 474.2 (MH+), 0.80 min.

1. customTo the crude reaction mixture
2. washwashed with saturated sodium bicarbonate (2×), water (5×), saturated salt solution, dried sodium sulfate
3. filtrationfiltered
4. concentrationThe solvent was concentrated off to constant mass under high vacuum
5. customto give the desire crude product which
6. custom474.2 (MH+), 0.80 min.