反应详情

温度

80 °C

To a solution of 5-(2-benzyloxy-4-iodophenyl)-1,1-dioxo-2-(2-trimethylsilanylethyl)-1,2,5-thiadiazolidin-3-one (100 mg, 0.183 mmol) in acetonitrile (2 mL) is added 1-benzenesulfonyl-2-vinylpyrrolidine (43 mg, 0.183 mmol), NEt3 (0.038 mL, 0.274 mmol), Pd(OAc)2 (2 mg, 0.034 mmol), and 2-(di-t-butylphosphino)biphenyl (4 mg) and the mixture stirred at 80° C. for 48 h. The reaction is cooled to RT and partitioned between 1N HCl and EtOAc. The organic phase is washed with brine and dried over magnesium sulfate. The solvent is removed under reduced pressure and the crude material purified by column chromatography using a gradient of 10-25% EtOAc/hexane to afford the title compound.

1. temperatureThe reaction is cooled to RT
2. custompartitioned between 1N HCl and EtOAc
3. washThe organic phase is washed with brine
4. dry with materialdried over magnesium sulfate
5. customThe solvent is removed under reduced pressure
6. customthe crude material purified by column chromatography