HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 22955954, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | 2,5-Difluoro-4-methylbenzoic acid | HCID 13657451 | — |
| Product | HCID 22955954 | HCID 22955954 | 95% |
Reaction Steps
To a solution of 2,5-difluoro-4-methylbenzoic acid (5 g, 2.904 mmol) in ethanol (100 mL) was added concentrated sulfuric acid (1 mL). The reaction mixture was stirred at reflux for 18 hours. LCMS showed complete consumption of starting material, so the solvents were removed in vacuo and the resulting residue redissolved in EtOAc (50 mL), and washed with saturated aqueous sodium bicarbonate. The organic layer was separated, and the aqueous layer extracted with EtOAc (2×50 mL). The combined organics were dried over sodium sulfate and evaporated to yield the title compound as a pale yellow oil (5.502 g, 95%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09102621B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-abaed093d29d477ba3963d7f1a4923c6 |
| Source note | uspto-grants-2015_08 |