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Sodium Carbonate → Methyl 6-(2-fluoro-5-formylphenyl)picolinate

HRID 2046879
Notes
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Reaction equation

HRID 2046879 reaction equation
Br[C:2]1[N:7]=[C:6]([C:8]([O:10][CH3:11])=[O:9])[CH:5]=[CH:4][CH:3]=1.[F:12][C:13]1[CH:18]=[CH:17][C:16]([CH:19]=[O:20])=[CH:15][C:14]=1B(O)O.C([O-])([O-])=O.[Na+].[Na+]>COCCOC.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:12][C:13]1[CH:18]=[CH:17][C:16]([CH:19]=[O:20])=[CH:15][C:14]=1[C:2]1[N:7]=[C:6]([C:8]([O:10][CH3:11])=[O:9])[CH:5]=[CH:4][CH:3]=1
ParticipantsConditionsProcedureSources & evidenceReaction notes

Participants

6

Reactant 3

HCID 10340Sodium CarbonateHCID 2763240(2-Fluoro-5-formylphenyl)boronic acidHCID 16217886Methyl 6-bromopyridine-2-carboxylate

Product 1

HCID 59226430Methyl 6-(2-fluoro-5-formylphenyl)picolinate

Reagents, catalysts & solvents 2

HCID 178418807HCID 178418807, compoundCatalyst
HCID 8071
1,2-Dimethoxyethane
Solvent

Conditions

Temperature
120 °C

Procedure

To a solution of methyl 6-bromopicolinate (1.0 equiv.) in DME (0.03 M) in a microwave vial was added Pd(dppf)Cl2-DCM (0.05 equiv.), 2-fluoro-5-formylphenylboronic acid (1.5 equiv.) and 2M Na2CO3 (2 equiv.). The reagents were heated to 120° C. for 20 min. A mixture of the desired product and the corresponding carboxylic acid was detected by LC/MS, the reaction was diluted with ethyl acetate, washed with HCl (pH=5), the acidic phase was extracted with ethyl acetate, the combined organic layers were dried with magnesium sulfate, filtered, and concentrated in vacuo to provide a light brown solid. The solid was dissolved in MeOH and treated with 3 equiv. of TMS-diazomethane at room temperature. Upon complete conversion of the carboxylic acid to the corresponding methyl ester, the reaction was concentrated in vacuo and the crude material was purified via silica gel column chromatography (ISCO) eluting with 30% ethyl acetate in hexanes to provide methyl 6-(2-fluoro-5-formylphenyl)picolinate as a yellow solid in 58% yield. LC/MS=260.0 (M+H), Rt=0.70 min.

Sources & evidence

ORD record
ord-b9cda8f218e8448ebf265ce4ad88d16b
Source dataset
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08592455B2

Reaction notes

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On this pageParticipantsConditionsProcedureSources & evidenceReaction notes