反应详情

温度

60 °C

Compound 137 (50 mg, 0.16 mmol), (5-tert-butyl-2-m-tolyl-2H-pyrazol-3-yl)-carbamic acid 2,2,2-trichloro-ethyl ester (80 mg, 0.20 mmol), and DIEA (0.08 mL, 0.49 mmol) were suspended in DMSO (2 mL), and stirred overnight at 60° C. The reaction solution 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 25 to 100% EtOAc in hexanes to provide 230 (22 mg, 24% yield) as a tan solid. LC-MS (M+H=559, obsd.=559).

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