반응 #612896

반응 방정식

TFA

6-chloro-N-(4-(chlorodifluoromethoxy)phenyl)-5-(1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-5-yl)nicotinamide

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title product

6-Chloro-N-(4-(chlorodifluoromethoxy)phenyl)-5-(1H-pyrazol-5-yl)nicotinamide

용매

DCM

반응 조건

후처리

1. 1
   기타The solvent was evaporated off under reduced pressure
2. 2
   workup.DISSOLUTIONthe residue was dissolved in EtOAc (150 mL)
3. 3
   세척washed with aq. sat. NaHCO3 solution (2×50 mL) and water (2×50 mL)
4. 4
   건조dried over Na2SO4
5. 5
   기타the solvent was evaporated off under reduced pressure
6. 6
   기타to give a residue
7. 7
   기타was crystallized from iPr2O/EtOAc

실험 절차

TFA (7.3 mL) was added to a solution of 6-chloro-N-(4-(chlorodifluoromethoxy)phenyl)-5-(1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-5-yl)nicotinamide (Stage 48.2, 1.285 g, 2.366 mmol) in DCM (20 mL) and the RM was stirred at RT. The solvent was evaporated off under reduced pressure and the residue was dissolved in EtOAc (150 mL), washed with aq. sat. NaHCO3 solution (2×50 mL) and water (2×50 mL) dried over Na2SO4 and the solvent was evaporated off under reduced pressure to give a residue was crystallized from iPr2O/EtOAc to give the title product as a white solid. HPLC (Condition 7) tR=6.797 min, UPLC-MS (Condition 3) tR=1.05-min, m/z=398.9/401.0 [M+H]+.

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