HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Peroxide → HCID 10420120, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Ethyl pyruvate | HCID 12041 | — |
| Reactant | 4-Acetylpyridine | HCID 14282 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10420120 | HCID 10420120 | 24.2% |
Reaction Steps
30% Hydrogen peroxide (130 ml) was added to ethyl pyruvate (216 g) at -5° to 5° C. with stirring. This solution was then added to a mixture of 4-acetylpyridine (15.0 g), concentrated sulfuric acid (12.4 g), ferrous sulfate heptahydrate (345 g), dichloromethane (1.5 l) and water (100 ml) at the same temperature with stirring. After further stirring for 30 minutes, the resulting organic layer was separated. The solution was washed with aqueous sodium sulfite and then water, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by silica gel column chromatography by eluting with a mixture of ethyl acetate and toluene (1:20) to give ethyl 4-acetyl-2-pyridinecarboxylate (5.79 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05371097 |
| Source dataset | uspto-grants-1994_12 |
| ORD ID | ord-9d35363ceaad4db190661363cfc809f8 |
| Source note | uspto-grants-1994_12 |