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2-Aminopyridine → 5-[3-(2-Chloro-4-pyrimidinyl)imidazo[1,2-a]pyridin-2-yl]-2-(methyloxy)-benzonitrile

HRID 419306
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HRID 419306 반응식
[Cl:1][C:2]1[N:7]=[C:6]([CH2:8][C:9]([C:11]2[CH:12]=[CH:13][C:14]([O:19][CH3:20])=[C:15]([CH:18]=2)[C:16]#[N:17])=O)[CH:5]=[CH:4][N:3]=1.Cl[C:22]1[N:27]=[C:26](/[CH:28]=[C:29](/[C:31]2C=CC(OC)=C(C=2)C#N)\O)C=C[N:23]=1.C1C(=O)N(Br)C(=O)C1.NC1C=CC=CN=1.C([O-])(O)=O.[Na+]>C(Cl)Cl>[Cl:1][C:2]1[N:7]=[C:6]([C:8]2[N:27]3[CH:26]=[CH:28][CH:29]=[CH:31][C:22]3=[N:23][C:9]=2[C:11]2[CH:12]=[CH:13][C:14]([O:19][CH3:20])=[C:15]([CH:18]=2)[C:16]#[N:17])[CH:5]=[CH:4][N:3]=1
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HCID 104392-AminopyridineHCID 67184N-bromobutanimideHCID 516892Sodium BicarbonateHCID 594527625-[(2-Chloro-4-pyrimidinyl)acetyl]-2-(methyloxy)benzonitrileHCID 1360784795-[(Z)-2-(2-chloro-4-pyrimidinyl)-1-hydroxyethenyl]-2-(methyloxy)benzonitrile

생성물 1

HCID 59452778
5-[3-(2-Chloro-4-pyrimidinyl)imidazo[1,2-a]pyridin-2-yl]-2-(methyloxy)-benzonitrile
수율 65%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
65 °C

실험 절차

To a tautomeric mixture of 5-[(2-chloro-4-pyrimidinyl)acetyl]-2-(methyloxy)benzonitrile and 5-[(Z)-2-(2-chloro-4-pyrimidinyl)-1-hydroxyethenyl]-2-(methyloxy)benzonitrile (2.87 g, 10.0 mmol) in DCM (250 mL) was added NBS (1.78 g, 10.0 mmol) in one portion. Upon completion by TLC, the reaction was concentrated. The residue was taken up in dioxane (100 mL) and 2-aminopyridine (2.89 g, 30.7 mmol) was added. The reaction was stirred at 65° C. overnight. The reaction was poured into half saturated NaHCO3, extracted with DCM and EtOAc, dried (MgSO4), concentrated and triturated with diethyl ether to provide the title compound (2.36 g, 6.50 mmol, 65%). 1H NMR (400 MHz, DMSO-d6) δ ppm 3.96 (s, 3H), 7.18-7.25 (m, 2H), 7.33 (d, J=9.0 Hz, 1H), 7.52-7.58 (m, 1H), 7.77 (d, J=9.0 Hz, 1H), 7.92 (dd, J=8.8, 2.4 Hz, 1H), 8.00 (d, J=2.2 Hz, 1H), 8.56 (d, J=5.5 Hz, 1H), 9.34-9.39 (m, 1H).

후처리

  1. concentrationUpon completion by TLC, the reaction was concentrated
  2. extractionextracted with DCM and EtOAc
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated
  5. customtriturated with diethyl ether

출처 및 근거

ORD 기록
ord-e6278c44c88347c3a67109938e2b9762
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08093239B2

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