反应详情

温度

10 °C

2-Bromobenzenesulfonyl chloride (1.0 g, 3.91 mmol) and triethylamine (455 mg, 0.63 mL, 4.5 mmol) were dissolved in THF (15 mL), and the mixture was cooled to 10° C. Dibenzylamine (849 mg, 0.83 mL, 4.3 mmol) was then added dropwise. The cooling bath was removed, and the reaction mixture was stirred for 10 h at rt and then an additional 6 h at 60° C. After cooling to rt, the solvent was removed under reduced pressure, and ethyl acetate was added. The organic layer was successively washed with 1N HCl, water, semi-saturated aq Na2CO3 solution, water, and brine. After drying with Na2SO4 and filtration, the solvent was removed under reduced pressure to afford the title compound as off-white crystals (1.44 g, 88%). 1H NMR (400 MHz, CDCl3) δ 4.42 (s, 4H), 7.08 (m, 4H), 7.27 (m, 6H), 7.41 (m, 2H), 7.78 (d, 1H), 8.19 (d, 1H).

1. customThe cooling bath was removed
2. customan additional 6 h
3. customat 60° C
4. temperatureAfter cooling to rt
5. customthe solvent was removed under reduced pressure, and ethyl acetate
6. additionwas added
7. washThe organic layer was successively washed with 1N HCl, water, semi-saturated aq Na2CO3 solution, water, and brine
8. dry with materialAfter drying with Na2SO4 and filtration
9. customthe solvent was removed under reduced pressure