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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 919798Generated: October 31, 2026

Hydrochloric Acid → 1-Benzyl-5-(5-fluoro-pyridin-3-yl)-8-hydroxy-2-oxo-1,2-dihydro-[1,6]naphthyridine-7-carboxylic acid methyl ester

https://huagongshe.com/reaction/919798

Reaction equation

Participants

RoleNameHCIDCharge
ReactantHydrochloric AcidHCID 313—
ReactantCesium carbonateHCID 10796—
Reactant(5-Fluoropyridin-3-yl)boronic acidHCID 44717403—
Reactant1-Benzyl-5-bromo-8-hydroxy-2-oxo-1,2-dihydro-[1,6]naphthyridine-7-carboxylic acid methyl esterHCID 86714119—
CatalystHCID 178418397HCID 178418397—
SolventDimethylformamideHCID 6228—
SolventEthyl AcetateHCID 8857—
SolventSodium chloride; waterHCID 57417360—
Product1-Benzyl-5-(5-fluoro-pyridin-3-yl)-8-hydroxy-2-oxo-1,2-dihydro-[1,6]naphthyridine-7-carboxylic acid methyl esterHCID 6829735761.7%

Reaction Conditions

Temperature100 °C

Reaction Steps

A mixture of 1-benzyl-5-bromo-8-hydroxy-2-oxo-1,2-dihydro-[1,6]naphthyridine-7-carboxylic acid methyl ester (70 mg, 0.18 mmol), 5-fluoro-pyridine-3-boronic acid (30 mg, 0.22 mmol), Pd(PPh3)4 (21 mg, 0.018 mmol) and Cs2CO3 (117 mg, 0.36 mmol) in DMF (4 mL) was heated at 100° C. for 16 h under nitrogen atmosphere. After cooling to r.t., EtOAc (50 mL) and brine (10 mL) were added. 1 M HCl was added until pH about 4. The aqueous layer was extracted with additional EtOAc, and the organic layers were combined, washed with water, and dried over MgSO4. After evaporating the solvent, the crude product was purified by silica gel chromatography (0-70% EtOAc/hexanes+2% AcOH) to give 45 mg of the title compound. MS: (+) m/z 406.33 (M+1).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09271970B2
Source datasetuspto-grants-2016_03
ORD IDord-fdfd8ed9e8dc4da9958989e6bdc65782
Source noteuspto-grants-2016_03