HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → Ethyl 3-hydroxy-5-methoxypicolinate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | 3-Hydroxy-5-methoxypicolinic acid | HCID 21543008 | — |
| Catalyst | Sulfuric Acid | HCID 1118 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Ethyl 3-hydroxy-5-methoxypicolinate | HCID 66962131 | 76% |
Reaction Steps
3-hydroxy-5-methoxypicolinic acid (200 mg, 1.18 mmol) was dissolved in ethanol (10 mL). To the mixture was added one drop of sulfuric acid. The mixture was refluxed with stirring for 3 days. After cooling to room temperature, the mixture was concentrated in vacuo to afford an oil. The residual oil was dissolved in ethyl acetate and washed with aq. sodium bicarbonate and brine. The extract was dried over sodium sulfate and concentrated in vacuo to afford an oil. The residual oil was purified by silica gel column chromatography (ethyl acetate/hexane 1:3 to 1:1) to afford 178 mg (76%) of the title compound as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08809380B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-912e881fe80d4fdbb15e85794f4619c3 |
| Source note | uspto-grants-2014_08 |