反应详情

To a solution of 1-(2-chloro-phenyl)-5-[4-(1,2,3,6-tetrahydropyridin-4-yl)-phenyl]-3-pentafluoroethyl-4,5-dihydro-1H-pyrazole trifluoroacetate (80.0 mg, 0.14 mmol) prepared in Example 10 in dichloromethane (1.0 mL), was added triethylamine (59.0 uL, 0.43 mmol). Methanesulfonyl chloride (16.5 uL, 0.22 mmol) was dropwisely added at 0° C. to the reaction mixture, which was then stirred at room temperature for 2 hours. Distilled water was added to the reaction mixture, which was then extracted with ethyl acetate. The extract was washed with brine, dried on anhydrous magnesium sulfate, and then concentrated under reduced pressure to give a yellow liquid residue. The resulting residue was purified by silica gel column chromatography (eluent: ethyl acetate/n-hexane=1/2) to give 50.8 mg of the titled compound as a pale yellow liquid.

1. extractionwas then extracted with ethyl acetate
2. washThe extract was washed with brine
3. dry with materialdried on anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customto give a yellow liquid residue
6. customThe resulting residue was purified by silica gel column chromatography (eluent: ethyl acetate/n-hexane=1/2)