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Hydrochloric Acid → 1-(6-(5-(2,6-difluorophenyl)-1H-indazol-3-yl)pyrazin-2-yl)piperidin-3-amine

HRID 1529282
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HRID 1529282 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[C:9]1[CH:10]=[C:11]2[C:15](=[CH:16][CH:17]=1)[N:14](C1CCCCO1)[N:13]=[C:12]2[C:24]1[N:29]=[C:28]([N:30]2[CH2:35][CH2:34][CH2:33][CH:32]([NH:36]C(=O)OC(C)(C)C)[CH2:31]2)[CH:27]=[N:26][CH:25]=1.Cl>CCOCC.O.C([O-])([O-])=O.[K+].[K+]>[F:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([F:1])[C:3]=1[C:9]1[CH:10]=[C:11]2[C:15](=[CH:16][CH:17]=1)[NH:14][N:13]=[C:12]2[C:24]1[N:29]=[C:28]([N:30]2[CH2:35][CH2:34][CH2:33][CH:32]([NH2:36])[CH2:31]2)[CH:27]=[N:26][CH:25]=1
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참가 물질

6

반응물 2

HCID 313Hydrochloric AcidHCID 67959937tert-butyl 1-(6-(5-(2,6-difluorophenyl)-1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-3-yl)pyrazin-2-yl)piperidin-3-ylcarbamate

생성물 1

HCID 679601391-(6-(5-(2,6-difluorophenyl)-1H-indazol-3-yl)pyrazin-2-yl)piperidin-3-amine

시약·촉매·용매 3

HCID 962Water용매HCID 3283Diethyl Ether용매2회
HCID 11430Potassium Carbonate용매

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온도
80 °C

실험 절차

To a solution of tert-butyl 1-(6-(5-(2,6-difluorophenyl)-1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-3-yl)pyrazin-2-yl)piperidin-3-ylcarbamate (350 mg, 0.592 mmol) in Et2O (6 mL) was added HCl in Et2O (6 mL). The reaction mixture was heated at 80° C. overnight and cooled to RT. The resulting mixture was diluted with water and neutralized with K2CO3. The resulting precipitate was collected by filtration, washed with water and a mixture of EtOH/EtOA (1:10), and dried overnight to give 1-(6-(5-(2,6-difluorophenyl)-1H-indazol-3-yl)pyrazin-2-yl)piperidin-3-amine MS (ESI, pos. ion) m/z: 407 (M+1).

후처리

  1. temperaturecooled to RT
  2. filtrationThe resulting precipitate was collected by filtration
  3. washwashed with water
  4. additiona mixture of EtOH/EtOA (1:10)
  5. customdried overnight

출처 및 근거

ORD 기록
ord-ce80bb2c46664652b1007e924b484a7d
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09090593B2

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