Trifluoroacetic acid → N-((3-fluoro-2'-(trifluoromethyl)-2,4'-bipyridin-5-yl)methyl)-5-(piperazin-1-yl)picolinamide

HRID 711259노트

반응식

HRID 711259 반응식
[F:1][C:2]1[C:3]([C:31]2[CH:36]=[CH:35][N:34]=[C:33]([C:37]([F:40])([F:39])[F:38])[CH:32]=2)=[N:4][CH:5]=[C:6]([CH2:8][NH:9][C:10]([C:12]2[N:17]=[CH:16][C:15]([N:18]3[CH2:23][CH2:22][N:21](C(OC(C)(C)C)=O)[CH2:20][CH2:19]3)=[CH:14][CH:13]=2)=[O:11])[CH:7]=1.C(O)(C(F)(F)F)=O>ClCCl>[F:1][C:2]1[C:3]([C:31]2[CH:36]=[CH:35][N:34]=[C:33]([C:37]([F:40])([F:38])[F:39])[CH:32]=2)=[N:4][CH:5]=[C:6]([CH2:8][NH:9][C:10](=[O:11])[C:12]2[CH:13]=[CH:14][C:15]([N:18]3[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]3)=[CH:16][N:17]=2)[CH:7]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 68079197Tert-butyl 4-(6-((3-fluoro-2'-(trifluoromethyl)-2,4'-bipyridin-5-yl)methylcarbamoyl)pyridin-3-yl)piperazine-1-carboxylate

생성물 1

HCID 68079457N-((3-fluoro-2'-(trifluoromethyl)-2,4'-bipyridin-5-yl)methyl)-5-(piperazin-1-yl)picolinamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of tert-butyl 4-(6-((3-fluoro-2′-(trifluoromethyl)-2,4′-bipyridin-5-yl)methylcarbamoyl)pyridin-3-yl)piperazine-1-carboxylate 49-5 (106 mg, 0.21 mmol) in dichloromethane (2 mL) was added TFA (1 mL) dropwise. The mixture was stirred at room temperature for 2 hours, and the solvents were removed by rotary evaporation. The residue was dissolved in ethyl acetate (100 mL), washed with saturated aqueous NaHCO3 solution, H2O and brine, dried over Na2SO4 and concentrated to dryness by rotary evaporation to give N-((3-fluoro-2′-(trifluoromethyl)-2,4′-bipyridin-5-yl)methyl)-5-(piperazin-1-yl)picolinamide 49-6 as yellow solid. MS m/z 461.2 (M+1)

후처리

  1. customthe solvents were removed by rotary evaporation
  2. dissolutionThe residue was dissolved in ethyl acetate (100 mL)
  3. washwashed with saturated aqueous NaHCO3 solution, H2O and brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated to dryness by rotary evaporation

출처 및 근거

ORD 기록
ord-a6692e020ecd4fcda6339f253b15fc42
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181235B2

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