反应详情

温度

0 °C

1-(4′,6-Dichlorobiphenyl-3-yl)-N-(4-fluorobenzyl)methanamine (200 mg, 0.555 mmol, 1.0 eq) was dissolved in dry DCM and the resulting solution was stirred for 10 minutes and cooled to 0° C. Triethylamine (168 mg, 1.6 mmol, 3 eq) was added to the above solution and the mixture was stirred for 10 minutes. 3,5-Dichloro-2-hydroxybenzene-1-sulfonyl chloride dissolved in DCM was added slowly over a period of 10 minutes and the mixture was stirred for 4 h at ambient temperature. The solvent was evaporated under reduced pressure and the residue was purified by flash column chromatography on silica gel (60-120) eluting with 5-10% ethyl acetate/hexane to give the title compound (0.14 g, 46%). 1H NMR (400 MHz, CD3OD) δ 4.47 (s, 2H), 4.53 (s, 2H), 6.91-6.98 (m, 3H), 7.12-7.15 (m, 1H), 7.22-7.27 (m, 4H), 7.33-7.35 (d, 1H), 7.43-7.45 (d, 2H), 7.54 (d, 1H), 7.67 (d, 1H). MS (ESI): 583.8 (M−H)−.

1. stirringthe mixture was stirred for 10 minutes
2. additionwas added slowly over a period of 10 minutes
3. stirringthe mixture was stirred for 4 h at ambient temperature
4. customThe solvent was evaporated under reduced pressure
5. customthe residue was purified by flash column chromatography on silica gel (60-120)
6. washeluting with 5-10% ethyl acetate/hexane