反应详情

To a solution of compound 9 (100 mg, 0.27 mmol) in CH3CN (5 mL) was added K2CO3 (74 mg, 0.54 mmol). After addition, the resulting mixture was stirred at room temperature for 10 min. Then 1,1-difluoro-2-iodo-ethane (51.8 mg, 0.27 mmol) in CH3CN (5 mL) was added dropwise via a syringe with stirring. The mixture was stirred at 60° C. overnight. Then the mixture was filtered off, the filtrate was concentrated to give compound 10 (90 mg, 77%) as a white solid, which was used for the next step directly without purification. LC-MS tR=1.337 min in 2 min chromatography, MS (ESI) m/z 435.2 [M+H]+.

1. additionAfter addition
2. stirringwith stirring
3. stirringThe mixture was stirred at 60° C. overnight
4. filtrationThen the mixture was filtered off
5. concentrationthe filtrate was concentrated