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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 37489Generated: October 28, 2026

Dimethylformamide → HCID 135711048, compound

https://huagongshe.com/reaction/37489

Reaction equation

Participants

RoleNameHCIDCharge
ReactantDimethylformamideHCID 6228—
ReactantPhosphorus oxychlorideHCID 24813—
ReactantHCID 178470074HCID 178470074—
ProductHCID 135711048HCID 135711048—

Reaction Conditions

Temperature100 °C

Reaction Steps

In 2.5 ml of phosphorus oxychloride was suspended 130 mg of 3,4-diethoxycarbonyl-2-hydroxy-6-(4-hydroxyphenyl)-5-nitropyridine, whereto 0.4 ml of DMF was added. The mixture was heated at 100° C. for 30 minutes. Then, 0.4 ml of DMF was added and the mixture was heated for further 30 minutes. After the solvent was distilled off, ice-water was added, followed by neutralization with sodium hydrogencarbonate and extraction with ethyl acetate. After the organic layer was washed with water and a saturated aqueous solution of sodium chloride and dried, the solvent was distilled off. The residue was purified by silica gel column chromatography (eluent:ethyl acetate).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS05420275
Source datasetuspto-grants-1995_05
ORD IDord-1463a6523746465287afe05d588b267d
Source noteuspto-grants-1995_05