HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 86589855, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 11010838 | HCID 11010838 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86589855 | HCID 86589855 | 93.3% |
Reaction Steps
A mixture of ethyl 2-ethyl-3-(3-formyl-4-methoxyphenyl)propanoate (1.06 g, 4.01 mmol), hydroxylamine hydrochloride (293 mg, 4.22 mmol), pyridine (1 mL) and ethanol (20 mL) was refluxed for 6 hours. After cooling, the mixture was concentrated and the residue was dissolved in ethyl acetate, which was washed with 1 mol/L hydrochloric acid, saturated aqueous solution of sodium hydrogencarbonate and brine, dried over anhydrous sodium sulfate, and then concentrated. The residue was purified by silica gel column chromatography (eluent: n-hexane:ethyl acetate=6:1 v/v) to afford 1.00 g (89%) of the title compound as a pale yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07049342B2 |
| Source dataset | uspto-grants-2006_05 |
| ORD ID | ord-410f5fec491348f195ecf20c9dae3058 |
| Source note | uspto-grants-2006_05 |