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

HRID 419306
Notes
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Reaction equation

HRID 419306 reaction equation
[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
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 5

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

Product 1

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

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Conditions

Temperature
65 °C

Procedure

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).

Workup

  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

Sources & evidence

ORD record
ord-e6278c44c88347c3a67109938e2b9762
Source dataset
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08093239B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes