HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 54028213, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethyl Oxalate | HCID 7268 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-(4-Nitrophenyl)-3-buten-2-one | HCID 101924 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 54028213 | HCID 54028213 | 44.3% |
Reaction Steps
Ethanol (9.5 ml) is added to a suspension of 60% sodium hydride (26.3 g) in anhydrous ether (750 ml), and thereto is added dropwise a mixture of p-nitrobenzalacetone (130 g), diethyl oxalate (99.4 g) and anhydrous tetrahydrofuran (550 ml) at 5°-10° C. with agitation. The mixture is agitated at room temperature for one hour, and thereto is added 10% hydrochloric acid (350 ml). The precipitated yellow solid is collected by filtration, washed with ether and then recrystallized from acetone to give ethyl 6-(4-nitrophenyl)-2,4-dioxo-hex-5-enoate (87.8 g). M.P. 148.5°-153.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04332809 |
| Source dataset | uspto-grants-1982_06 |
| ORD ID | ord-56006cb5cd864212a21e8b5f3aae5bbc |
| Source note | uspto-grants-1982_06 |