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2-Bromo-5-methylpyridine → 5-methyl-N-(4-(3-(tetrahydro-2H-pyran-4-yl)pyridin-2-yloxy)phenyl)pyridin-2-amine

HRID 473642
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HRID 473642 반응식
[O:1]1[CH2:6][CH2:5][CH:4]([C:7]2[C:8]([O:13][C:14]3[CH:20]=[CH:19][C:17]([NH2:18])=[CH:16][CH:15]=3)=[N:9][CH:10]=[CH:11][CH:12]=2)[CH2:3][CH2:2]1.Br[C:22]1[CH:27]=[CH:26][C:25]([CH3:28])=[CH:24][N:23]=1.CC(C)([O-])C.[Na+]>CC(C1C=C(C(C)C)C(C2C(P(C3CCCCC3)C3CCCCC3)=C(OC)C=CC=2OC)=C(C(C)C)C=1)C.C1C=[C-]C(CCN)=CC=1.Cl[Pd+]>[CH3:28][C:25]1[CH:26]=[CH:27][C:22]([NH:18][C:17]2[CH:16]=[CH:15][C:14]([O:13][C:8]3[C:7]([CH:4]4[CH2:3][CH2:2][O:1][CH2:6][CH2:5]4)=[CH:12][CH:11]=[CH:10][N:9]=3)=[CH:20][CH:19]=2)=[N:23][CH:24]=1
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참가 물질

5

반응물 3

HCID 5642162-Bromo-5-methylpyridineHCID 23676156Sodium t-butoxideHCID 593271274-(3-(tetrahydro-2H-pyran-4-yl)pyridin-2-yloxy)aniline

생성물 1

HCID 593741535-methyl-N-(4-(3-(tetrahydro-2H-pyran-4-yl)pyridin-2-yloxy)phenyl)pyridin-2-amine

시약·촉매·용매 1

HCID 25112666BrettPhos Palladacycle촉매

반응 조건

온도
90 °C

실험 절차

A glass microwave reaction vessel was charged with 4-(3-(tetrahydro-2H-pyran-4-yl)pyridin-2-yloxy)aniline (0.167 g, 0.619 mmol), 2-bromo-5-methylpyridine (0.0888 g, 0.516 mmol), BrettPHOS precatalyst (8.26 mg, 10.32 μmol), and sodium tert-butoxide (0.124 g, 1.291 mmol). The flask was placed under vacuum then flushed with argon. Dioxane (1.7 mL) was added and the reaction was heated to 90° C. to stir overnight. After cooling to room temperature, the reaction mixture was concentrated and the crude product was adsorbed onto a plug of silica gel and chromatographed through a Biotage pre-packed silica gel column (40S), eluting with a gradient of 10% to 100% EtOAc in hexane, to provide 5-methyl-N-(4-(3-(tetrahydro-2H-pyran-4-yl)pyridin-2-yloxy)phenyl)pyridin-2-amine. MS (ESI, pos. ion) m/z: 362.1 (M+1). IC50 (uM) 0.002387.

후처리

  1. customA glass microwave reaction vessel
  2. customthen flushed with argon
  3. additionDioxane (1.7 mL) was added
  4. temperatureAfter cooling to room temperature
  5. concentrationthe reaction mixture was concentrated
  6. customchromatographed through a Biotage pre-packed silica gel column (40S)
  7. washeluting with a gradient of 10% to 100% EtOAc in hexane

출처 및 근거

ORD 기록
ord-f9f3bc2a2e6f4bf5a2202024b9c40f3e
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08637500B2

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