HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 135711048, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 178470074 | HCID 178470074 | — |
| Product | HCID 135711048 | HCID 135711048 | — |
Reaction Conditions
| Temperature | 100 °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
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05420275 |
| Source dataset | uspto-grants-1995_05 |
| ORD ID | ord-1463a6523746465287afe05d588b267d |
| Source note | uspto-grants-1995_05 |