反应 #1399739
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08039514B2
反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 2-Bromobenzenesulfonyl chloride (manufactured by Fluorochem Co., 25 g) was dissolved in tetrahydrofuran (40 mL), and under stirring at 0° C., 40% methylamine aqueous solution (TCI, 25 mL) was added dropwise thereto over ten minutes. After stirring the mixture at room temperature for 2 hours and 40 minutes, water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and the solvent was removed by distillation under reduced pressure. To the residues, hexane and a small amount of ethyl acetate were added, followed by stirring. Solids were filtered to obtain the target compound (23.26 g). over ten minutes After stirring the mixture at room temperature for 2 hours followed by extraction with ethyl acetate The organic layer was washed with brine dried over anhydrous sodium sulfate the solvent was removed by distillation under reduced pressure To the residues, hexane and a small amount of ethyl acetate were added by stirring Solids were filtered
来源 ID: ord-bc88a6d7871c4a87b298a5bcc8f35e91