反应详情

Compound 218 (25 mg, 0.07 mmol), 1-chloro-3-isocyanato-benzene (17 mg, 0.11 mmol), and DIEA (0.04 mL, 0.22 mmol) were dissolved in dioxane (2 mL) and stirred and stirred for 30 minutes at 100° C. in microwave. The reaction mixture was diluted with H2O/EtOAc, 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 50 to 100% EtOAc in hexanes to provide 221 (8 mg, 22% yield) as a tan solid. LC-MS (M+H=499, obsd.=499).

1. stirringstirred for 30 minutes at 100° C. in microwave
2. filtrationfiltered through an Extrelut column
3. washThe column was washed with EtOAc
4. concentrationthe filtrate was concentrated
5. customThe crude product was purified via Biotage
6. washeluting with a gradient of 50 to 100% EtOAc in hexanes