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Phosgene → N-(1-methyl-1H-indazol-4-yl)-4-[4-(trifluoromethyl)-2-pyridinyl]-1-piperazinecarboxamide

HRID 586083
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HRID 586083 반응식
[CH3:1][N:2]1[C:10]2[CH:9]=[CH:8][CH:7]=[C:6]([NH2:11])[C:5]=2[CH:4]=[N:3]1.[C:12](Cl)(Cl)=[O:13].C(NC(C)C)(C)C.[F:23][C:24]([F:38])([F:37])[C:25]1[CH:30]=[CH:29][N:28]=[C:27]([N:31]2[CH2:36][CH2:35][NH:34][CH2:33][CH2:32]2)[CH:26]=1>C1(C)C=CC=CC=1>[CH3:1][N:2]1[C:10]2[C:5](=[C:6]([NH:11][C:12]([N:34]3[CH2:35][CH2:36][N:31]([C:27]4[CH:26]=[C:25]([C:24]([F:38])([F:23])[F:37])[CH:30]=[CH:29][N:28]=4)[CH2:32][CH2:33]3)=[O:13])[CH:7]=[CH:8][CH:9]=2)[CH:4]=[N:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6371PhosgeneHCID 7912DiisopropylamineHCID 1538381H-Indazol-4-amine, 1-methyl-HCID 112184921-[4-(Trifluoromethyl)pyridin-2-yl]piperazine

생성물 1

HCID 22337654N-(1-methyl-1H-indazol-4-yl)-4-[4-(trifluoromethyl)-2-pyridinyl]-1-piperazinecarboxamide

시약·촉매·용매 1

HCID 1140
Toluene
용매

실험 절차

1-Methyl-1H-indazol-4-amine (560 mg, 3.81 mmol) in toluene (20 mL) was treated with 20% phosgene solution (2.5 mL) and refluxed overnight. The mixture was allowed to cool to ambient temperature and was concentrated under reduced pressure. The residue was taken up in THF (20 mL) and treated with diisopropylamine (5 mL) and 1-[4-(trifluoromethyl)-2-pyridinyl]piperazine (450 mg, 1.95 mmol). The mixture was refluxed overnight, allowed to cool to ambient temperature, and concentrated under reduced pressure. The residue was purified by flash chromatography (97:3 CH2Cl2:CH3OH to 95:5 CH2Cl2:CH3OH) to provide the title compound. The corresponding hydrochloride salt was prepared by treatment with methanolic HCl. 1H NMR (300 MHz, d6-DMSO) δ 8.78 (s, 1H), 8.44 (m, 1H), 8.07 (d, J=1.0 Hz, 1H), 7.83 (m, 1H), 7.19-7.31 (m, 3H), 7.02 (d, 9.2 Hz, 1H), 4.00 (s, 3H), 3.74 (m, 4H), 3.63 (m, 4H); MS (ESI+) m/z 405 (M+H)+.

후처리

  1. temperaturerefluxed overnight
  2. concentrationwas concentrated under reduced pressure
  3. temperatureThe mixture was refluxed overnight
  4. temperatureto cool to ambient temperature
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by flash chromatography (97:3 CH2Cl2:CH3OH to 95:5 CH2Cl2:CH3OH)

출처 및 근거

ORD 기록
ord-df41d33ce34b487e88b7b55d84e7c2f8
출처 데이터셋
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06933311B2

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