Trifluoroacetic acid → 6-chloro-N-(4-(chlorodifluoromethoxy)phenyl)-5-(1H-pyrazol-5-yl)nicotinamide

HRID 525714노트

반응식

HRID 525714 반응식
C(O)(C(F)(F)F)=O.[Cl:8][C:9]1[C:28]([C:29]2[N:33](C3CCCCO3)[N:32]=[CH:31][CH:30]=2)=[CH:27][C:12]([C:13]([NH:15][C:16]2[CH:21]=[CH:20][C:19]([O:22][C:23]([Cl:26])([F:25])[F:24])=[CH:18][CH:17]=2)=[O:14])=[CH:11][N:10]=1>C(Cl)Cl>[Cl:8][C:9]1[C:28]([C:29]2[NH:33][N:32]=[CH:31][CH:30]=2)=[CH:27][C:12]([C:13]([NH:15][C:16]2[CH:21]=[CH:20][C:19]([O:22][C:23]([Cl:26])([F:25])[F:24])=[CH:18][CH:17]=2)=[O:14])=[CH:11][N:10]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 867026376-chloro-N-(4-(chlorodifluoromethoxy)phenyl)-5-(1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-5-yl)nicotinamide

생성물 1

HCID 722015896-chloro-N-(4-(chlorodifluoromethoxy)phenyl)-5-(1H-pyrazol-5-yl)nicotinamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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]+.

후처리

  1. customThe solvent was evaporated off under reduced pressure
  2. dissolutionthe residue was dissolved in EtOAc (150 mL)
  3. washwashed with aq. sat. NaHCO3 solution (2×50 mL) and water (2×50 mL)
  4. dry with materialdried over Na2SO4
  5. customthe solvent was evaporated off under reduced pressure
  6. customto give a residue
  7. customwas crystallized from iPr2O/EtOAc

출처 및 근거

ORD 기록
ord-37d648f6d9b741a59e61e827d10e1624
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09340537B2

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