HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → Ethyl 4-fluoro-3-hydroxybenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 4-Fluoro-3-hydroxybenzoic acid | HCID 593635 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Ethyl 4-fluoro-3-hydroxybenzoate | HCID 18007712 | 93% |
Reaction Steps
To a solution of 4-fluoro-3-hydroxy-benzoic acid (2 g, 12.81 mmol) in absolute ethanol (30 ml) was added thionyl chloride (1 ml) drop wise at 0° C. After refluxing for overnight, the solvents were driven off, the residue was dissolved in dichloromethane (50 ml), cooled on ice bath, neutralized slowly with 1M NaHCO3, and the layers were separated. The aqueous layer was extracted with dichloromethane (50 ml) for one more time. Combined organic extracts were dried (Na2SO4), filtered, concentrated, and purified by flash column chromatography using dichloromethane to yield 2.2 g (93%) of product. MS (ESI+) m/z 185 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07704997B1 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-1c49cd5907c24c72bec718bcbd578f2d |
| Source note | uspto-grants-2010_04 |