反应详情

温度

110 °C

A suspension of 5-methyl-1-[4-(trifluoromethyl)phenyl]-1H-pyrazole-4-carboxamide (212 mg), 5-bromo-2-(3,6-dihydro-2H-pyran-4-yl)-3-methylpyridine (200 mg) described in Reference Example 135, 2-(di-tert-butylphosphino)-3,4,5,6-tetramethyl-2′,4′,6′-triisopropyl-1,1′-biphenyl (19 mg), tris(dibenzylideneacetone)dipalladium (0) (7.2 mg) and tripotassium phosphate (200 mg) in tert-butanol (3 ml) was stirred at 110° C. After the reaction, the reaction solution was left stand, diluted with chloroform and filtered through Celite. The organic layer was washed with water and saturated brine successively, dried over anhydrous sodium sulfate and concentrated. The resulting residue was purified with a silica gel column chromatography (chloroform/methanol), washed with hot ethanol and the resulting solid was filtered and dried at 60° C. in vacuo to give the titled compound (202 mg) as a white solid.

1. customAfter the reaction
2. waitthe reaction solution was left stand
3. filtrationfiltered through Celite
4. washThe organic layer was washed with water and saturated brine successively
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated
7. customThe resulting residue was purified with a silica gel column chromatography (chloroform/methanol)
8. washwashed with hot ethanol
9. filtrationthe resulting solid was filtered
10. customdried at 60° C. in vacuo