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3-Bromopyridine → 3-(2-Fluorophenyl)pyridine

HRID 1061769
Notes
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Reaction equation

HRID 1061769 reaction equation
Br[C:2]1[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=1.[F:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1B(O)O.[F-].[K+].C(P(C(C)(C)C)C(C)(C)C)(C)(C)C>C1COCC1.O1CCOCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[F:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[C:2]1[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

8

Reactant 4

HCID 122863-BromopyridineHCID 83681Tris(1,1-dimethylethyl)phosphineHCID 522689Potassium FluorideHCID 27343542-Fluorophenylboronic acid

Product 1

HCID 132706453-(2-Fluorophenyl)pyridine

Reagents, catalysts & solvents 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
Catalyst
HCID 8028TetrahydrofuranSolvent
HCID 312751,4-DioxaneSolvent

Procedure

A mixture of 3-bromopyridine (3.37 mL, 5.53 g, 35 mmol), 2-fluorobenzeneboronic acid (6.12 g, 43.8 mmol) and potassium fluoride (6.71 g, 116 mmol) in THF (50 mL) was degassed with nitrogen for 10 min. Tris(dibenzylideneacetone)dipalladium(0) (0.64 g, 0.70 mmol) and tri(tert-butyl)phosphine (7 mL of a 0.2 M solution in dioxane, 1.4 mmol) were added. A solid precipitated, giving a thick slurry which was stirred under nitrogen for 15 min, then at 50° C. for 30 min. After cooling to room temperature, the mixture was partitioned between ethyl acetate and water. The organic phase was washed with saturated sodium chloride solution, then was dried over magnesium sulfate and pre-adsorbed on to silica gel. Purification by flash chromatography on silica gel eluting with isohexane (+0.5% methanol +0.5% triethylamine) on a gradient of 20% to 40% ethyl acetate afforded 3-(2-fluorophenyl)pyridine as a pale yellow oil, which crystallised upon standing. δH (360 MHz, DMSO) 7.33-7.40 (2H, m), 7.46-7.55 (2H, m), 7.61 (1H, ddd, J 8, 8 and 2), 7.96-8.01 (1H, m), 8.61 (1H, dd, J 5 and 2), 8.77 (1H, s).

Workup

  1. customwas degassed with nitrogen for 10 min
  2. customA solid precipitated
  3. customgiving a thick slurry which
  4. waitat 50° C. for 30 min
  5. customthe mixture was partitioned between ethyl acetate and water
  6. washThe organic phase was washed with saturated sodium chloride solution
  7. dry with materialwas dried over magnesium sulfate and pre-adsorbed on to silica gel
  8. customPurification by flash chromatography on silica gel eluting with isohexane (+0.5% methanol +0.5% triethylamine) on a gradient of 20% to 40% ethyl acetate

Sources & evidence

ORD record
ord-77d0f0ce534140a292257b3e0bdacce1
Source dataset
uspto-grants-2005_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06960598B2

Reaction notes

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