Trifluoroacetic acid → HCID 57955166, 화합물

HRID 1094911노트

반응식

HRID 1094911 반응식
[NH2:1][C:2]1[C:7]2=[C:8]([C:27]3[CH:32]=[CH:31][C:30]([NH:33][C:34](=[O:47])[NH:35][C:36]4[CH:41]=[C:40]([C:42]([F:45])([F:44])[F:43])[CH:39]=[CH:38][C:37]=4[F:46])=[C:29]([F:48])[CH:28]=3)[C:9]([CH2:24][O:25][CH3:26])=[C:10]([CH:11]3[CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][CH2:12]3)[N:6]2[N:5]=[CH:4][N:3]=1.FC(F)(F)C(O)=O>C(Cl)Cl>[NH2:1][C:2]1[C:7]2=[C:8]([C:27]3[CH:32]=[CH:31][C:30]([NH:33][C:34]([NH:35][C:36]4[CH:41]=[C:40]([C:42]([F:45])([F:43])[F:44])[CH:39]=[CH:38][C:37]=4[F:46])=[O:47])=[C:29]([F:48])[CH:28]=3)[C:9]([CH2:24][O:25][CH3:26])=[C:10]([CH:11]3[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]3)[N:6]2[N:5]=[CH:4][N:3]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 66641290Tert-butyl 4-{4-amino-5-[3-fluoro-4-({[2-fluoro-5-(trifluoromethyl)phenyl]carbamoyl}amino)phenyl]-6-(methoxymethyl)pyrrolo[2,1-f][1,2,4]triazin-7-yl}piperidine-1-carboxylate

생성물 1

HCID 57955166HCID 57955166, 화합물수율 70.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a flask charged with tert-butyl 4-{4-amino-5-[3-fluoro-4-({[2-fluoro-5-(trifluoromethyl)phenyl]carbamoyl}amino)phenyl]-6-(methoxymethyl)pyrrolo[2,1-f][1,2,4]triazin-7-yl}piperidine-1-carboxylate was added methylene chloride (12.5 mL). To this suspension was added 12.5 mL of trifluoroacetic acid. The homogeneous solution was allowed to stir at rt under nitrogen for 17 hours. The reaction mixture was concentrated and the residue dissolved in EtOAc. The organic phase was washed with saturated sodium bicarbonate solution (2×), brine (1×), separated and the organic layer dried (Na2SO4). The organic layer was filtered, concentrated and left under vacuum overnight to yield the title compound (150 mg, 70.4% yield). 1H-NMR (DMSO-d6) MS [M+H]+=576; LCMS RT=2.51 min.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. dissolutionthe residue dissolved in EtOAc
  3. washThe organic phase was washed with saturated sodium bicarbonate solution (2×), brine (1×)
  4. customseparated
  5. dry with materialthe organic layer dried (Na2SO4)
  6. filtrationThe organic layer was filtered
  7. concentrationconcentrated
  8. waitleft under vacuum overnight

출처 및 근거

ORD 기록
ord-c66161c5b55443568f6211d8a91f6b49
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08133995B2

반응 노트

불러오는 중…