反应详情

温度

-78 °C

To a solution of 3-benzyloxy-4-[1,1,4-trioxo-5-(2-trimethylsilanylethyl)-1,2,5-thiadiazolidin-2-yl]-benzaldehyde (Example 81, step B) (75 mg, 0.17 mmol) in anhydrous THF (4 mL) at −78° C. is added dropwise 2-pyridyl magnesium bromide (0.25M in THF, 1.36 mL, 0.34 mmol). The reaction is stirred at −78° C. for 1 h, then is quenched with saturated NH4Cl. The mixture is extracted with EtOAc and the organic phase is dried over MgSO4. The solvent is removed under reduced pressure and the crude material is purified by column chromatography using a gradient of 0-50% EtOAc/hexane to afford the title compound as a colorless oil: (M−H)−=526.

1. customis quenched with saturated NH4Cl
2. extractionThe mixture is extracted with EtOAc
3. dry with materialthe organic phase is dried over MgSO4
4. customThe solvent is removed under reduced pressure
5. customthe crude material is purified by column chromatography