Triethylamine → 1-(2,4-difluoro-phenyl)-5-[3-(4-methanesulfonyl-piperazin-1-yl)-pyridin-5-yl]-3-pentafluoroethyl-4,5-dihydro-1H-pyrazole

1-(2,4-Difluoro-phenyl)-5-[3-(piperazin-1-yl)-pyridin-5-yl]-3-pentafluoroethyl-4,5-dihydro-1H-pyrazole hydrochloride (30.0 mg, 0.06 mmol) prepared in Example 170, triethylamine (42.3 uL, 0.30 mmol) and methanesulfonyl chloride (10.4 mg, 0.09 mmol) were added to dichloromethane (1.0 mL). The reaction mixture was stirred at room temperature for 1 hour, washed with distilled water, 1N hydrochloride, a saturated solution of sodium hydrogen carbonate, and 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=2/1) to give 15.0 mg of the titled compound as a yellow liquid.

1. washwashed with distilled water, 1N hydrochloride
2. dry with materiala saturated solution of sodium hydrogen carbonate, and brine, dried on anhydrous magnesium sulfate
3. concentrationconcentrated under reduced pressure
4. customto give a yellow liquid residue
5. customThe resulting residue was purified by silica gel column chromatography (eluent: ethyl acetate/n-hexane=2/1)

ORD 기록

ord-0b3a995ef27c426492184cf28a1c6973

출처 데이터셋

uspto-grants-2016_06

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US09376420B2