Back
HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 919853Generated: November 2, 2026

Hydrochloric Acid → HCID 136377235, compound

https://huagongshe.com/reaction/919853

Reaction equation

Participants

RoleNameHCIDCharge
ReactantHydrochloric AcidHCID 313—
ReactantEthyl AcetateHCID 8857—
Reactant4-(Tri-n-butylstannyl)pyridineHCID 2737318—
Reactant1-Benzyl-3-bromo-5-hydroxy-2-oxo-1,2-dihydro-[1,7]naphthyridine-6-carboxylic acid methyl esterHCID 68297477—
CatalystHCID 178418476HCID 178418476—
SolventDimethylformamideHCID 6228—
SolventSodium chloride; waterHCID 57417360—
ProductHCID 136377235HCID 13637723541.6%

Reaction Conditions

Temperature120 °C

Reaction Steps

A mixture of 1-benzyl-3-bromo-5-hydroxy-2-oxo-1,2-dihydro-[1,7]naphthyridine-6-carboxylic acid methyl ester (70 mg, 0.18 mmol), 4-(tributylstannyl)pyridine (99 mg, 0.27 mmol), and PdCl2(PPh3)2 (25 mg, 0.036 mmol) in DMF (4 mL) was heated at 120° C. under nitrogen atmosphere for 3 h. After the mixture was cooled to r.t., brine (10 mL) and EtOAc (40 mL) were added. 1 M HCl was added with stirring until pH was about 3-4. 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 in vacuo, the crude product was purified by silica gel chromatography (20-100% EtOAc/hexanes+2% AcOH) to give 29 mg of the title compound. MS: (+) m/z 388.33 (M+1).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09271970B2
Source datasetuspto-grants-2016_03
ORD IDord-dd4a8857c7c64f9cb9fe117b9c00ec02
Source noteuspto-grants-2016_03