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Sodium Carbonate → 3-Fluoro-6-methyl-2-(2,3,5-trifluorophenyl)pyridine

HRID 2046872
Notes
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Reaction equation

HRID 2046872 reaction equation
Br[C:2]1[C:7]([F:8])=[CH:6][CH:5]=[C:4]([CH3:9])[N:3]=1.[F:10][C:11]1[C:16]([F:17])=[CH:15][C:14]([F:18])=[CH:13][C:12]=1B(O)O.C(=O)([O-])[O-].[Na+].[Na+]>O1CCOCC1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].C(Cl)Cl>[F:8][C:7]1[C:2]([C:12]2[CH:13]=[C:14]([F:18])[CH:15]=[C:16]([F:17])[C:11]=2[F:10])=[N:3][C:4]([CH3:9])=[CH:5][CH:6]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 3

HCID 10340Sodium CarbonateHCID 40788432,3,5-Trifluorophenylboronic AcidHCID 248203182-Bromo-3-fluoro-6-methylpyridine

Product 1

HCID 592265243-Fluoro-6-methyl-2-(2,3,5-trifluorophenyl)pyridineYield 87%

Reagents, catalysts & solvents 2

HCID 178418807HCID 178418807, compound
Catalyst
HCID 312751,4-DioxaneSolvent

Conditions

Temperature
120 °C

Procedure

To a solution of 2-bromo-3-fluoro-6-methylpyridine (1.0 equiv.) in dioxane (0.2 M) was added 2,3,5-trifluorophenylboronic acid and Pd(dppf)Cl2-DCM (0.1 equiv.). Aqueous sodium carbonate (2M solution, 2.0 equiv.) was added and the reaction was heated in the microwave at 120° C. for 15 min. The solution was partitioned between ethyl acetate and sat. NaHCO3, the organic phase was washed with brine, dried with magnesium sulfate, filtered, and concentrated. The crude material was purified via silica gel column chromatography eluting with ethyl acetate and hexanes (1:3) to give 3-fluoro-6-methyl-2-(2,3,5-trifluorophenyl)pyridine in 87% yield. LC/MS=242.1 (M+H), Rt=0.98 min.

Workup

  1. customThe solution was partitioned between ethyl acetate and sat. NaHCO3
  2. washthe organic phase was washed with brine
  3. dry with materialdried with magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe crude material was purified via silica gel column chromatography
  7. washeluting with ethyl acetate and hexanes (1:3)

Sources & evidence

ORD record
ord-1a15be0a86c74af4b84977cbd2ad78b5
Source dataset
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08592455B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes