HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → HCID 66939284, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | ethyl 1H-pyrazole-4-carboxylate | HCID 142179 | — |
| Reactant | HCID 66939077 | HCID 66939077 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 66939284 | HCID 66939284 | 76.6% |
Reaction Steps
To a suspension of sodium hydride (60% in mineral oil, 0.08 g) in N,N-dimethylformamide (2 ml) was added ethyl 1H-pyrazole-4-carboxylate (0.21 g). After stirring at room temperature for 30 min, the compound (0.42 g) obtained in Example 105a was added to the reaction mixture. After stirring at room temperature for 2 hr, 10% aqueous citric acid solution and ethyl acetate were added to the reaction mixture. The ethyl acetate layer was separated, washed with saturated brine, dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate) to give the title compound (0.44 g) as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08461348B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-3624be0252f54fda92bdafc92c3a5965 |
| Source note | uspto-grants-2013_06 |