反应详情

温度

22 °C

Combine triethylamine (117.83 mL) and palladium 10% on charcoal (20.10 g) to a solution of [4-(6-cyano-2-methyl-pyrimidin-4-yl)oxyphenyl]methanesulfonamide (67 g, 211.35 mmoles) in a mixture of 1,4-dioxane (469 mL) and EtOH (201 mL; 159.05 g) in a PARR reactor. Maintain the mixture at 22° C. Seal the reactor and pressurize it with hydrogen (400 PSI). Shake the reactor for 18 h while maintaining it at 22° C. Thereafter open the reactor and filter of the solids. Rinse the solid residue with MeOH (1 L), a mixture of dioxane/MeOH 1:1 (1 L), and MeOH (3×1 L). Collect and concentrate the filtrate to provide a solid, Collect and dry the solid in a vacuum oven, (45° C., 15 mbar) to provide the title compound as yellow solid, 62.41 g, 77% yield. MS (m/z): 309 (M+1).

1. customSeal the reactor
2. temperatureShake the reactor for 18 h while maintaining it at 22° C
3. filtrationThereafter open the reactor and filter of the solids
4. washRinse the solid residue with MeOH (1 L)
5. additiona mixture of dioxane/MeOH 1:1 (1 L), and MeOH (3×1 L)
6. customCollect
7. concentrationconcentrate the filtrate
8. customto provide a solid
9. customCollect
10. customdry the solid in a vacuum oven, (45° C., 15 mbar)