反应详情

To a mixture of 4-(2-chloro-4-fluorobenzoyl)-5-(2,6-difluorophenyl)-1-methyl-1H-pyrazole-3-carbonitrile (i.e. the product of Example 10) (0.05 g, 0.13 mmol) in ethanol (2 mL) was added sodium borohydride (0.005 g, 0.13 mmol). The reaction was stirred for 30 minutes, and then hydrochloric acid (1 N) (0.5 mL) was added and the mixture was concentrated under reduced pressure. The resulting material was diluted with methylene chloride (5 mL) and filter through a Celite® (diatomaceous earth) extraction tube rinsing with methylene chloride (15 mL). The filtrate was concentrated under reduced pressure and the resulting material purified by flash chromatography on a silica gel, Varian Bond Elute SI® column (10 to 50% gradient of ethyl acetate in hexanes as eluant) to provide the title compound, a compound of the present invention, as a solid (0.03 g).

1. concentrationthe mixture was concentrated under reduced pressure
2. additionThe resulting material was diluted with methylene chloride (5 mL)
3. filtrationfilter through a Celite® (diatomaceous earth) extraction tube
4. washrinsing with methylene chloride (15 mL)
5. concentrationThe filtrate was concentrated under reduced pressure
6. customthe resulting material purified by flash chromatography on a silica gel, Varian Bond
7. washElute SI® column (10 to 50% gradient of ethyl acetate in hexanes as eluant)