反应详情

温度

100 °C

To a solution of 5-(2-benzyloxy-4-vinylphenyl)-1,1-dioxo-2-(2-trimethylsilanylethyl)-1,2,5-thiadiazolidin-3-one (Example 81, step A) (75 mg, 0.17 mmol) in acetonitrile (2 mL), in a pressure vessel, is added 2-bromo-6-methoxypyridine (32 mg, 0.17 mmol), NEt3 (0.05 mL, 0.34 mmol), Pd(OAc)2 (8 mg, 0.034 mmol), and 2-(di-t-butylphosphino)biphenyl (20 mg, 0.068 mmol). The vessel is sealed and stirred at 100° C. for 18 h. The reaction is cooled to RT and filtered through Celite. The solvent is removed under reduced pressure and the crude material purified by column chromatography using a gradient of 0-35% EtOAc/hexanes as eluent to afford the title compound as a yellow oil: (M+H)+=552.

1. customThe vessel is sealed
2. temperatureThe reaction is cooled to RT
3. filtrationfiltered through Celite
4. customThe solvent is removed under reduced pressure
5. customthe crude material purified by column chromatography