反应详情

温度

80 °C

Compound 137 (50 mg, 0.16 mmol), 2,3-dichloro-benzenesulfonyl chloride (45 mg, 0.18 mmol), and Et3N (0.07 mL, 0.49 mmol) were suspended in dioxane (2 mL), and stirred overnight at 80° C. The reaction mixture was acidified with 1M HCl, and filtered through an Extrelut column. The column was washed with EtOAc, and the filtrate was concentrated. The crude product was purified via Biotage eluting with a gradient of 25 to 100% EtOAc in hexanes to provide 173 (14 mg, 17% yield) as a white solid. LC-MS (M+H=512, obsd.=512).

1. filtrationfiltered through an Extrelut column
2. washThe column was washed with EtOAc
3. concentrationthe filtrate was concentrated
4. customThe crude product was purified via Biotage
5. washeluting with a gradient of 25 to 100% EtOAc in hexanes