反应详情

温度

-78 °C

To a mixture of 2-methyl-propane-2-sulfonic acid 1-(3-bromo-phenyl)-meth-(Z)-ylideneamide (2.16 g, 7.49 mmol) and (fluoromethylsulfonyl)benzene (1.31 g, 7.49 mmol) in THF (50 mL), cooled to −78° C., was added LiHMDS (1M in THF; 7.87 mL, 7.87 mmol). The reaction mixture was stirred for 40 min at −78° C., followed by quenching saturated aqueous NH4Cl (10 mL) at −78° C. The mixture was extracted with EtOAc (3×), dried over Na2SO4, filtered and concentrated in vacuo. Purification by flash column chromatography on silica gel (c-hexane/EtOAc 3:1) afforded the title compound. MS (LC/MS): 462/464 [M+H]+; tR (HPLC conditions f): 2.20 min.

1. customby quenching saturated aqueous NH4Cl (10 mL) at −78° C
2. extractionThe mixture was extracted with EtOAc (3×)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customPurification by flash column chromatography on silica gel (c-hexane/EtOAc 3:1)