HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → Methyl 2-methyl-1-benzofuran-5-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 2-methyl-1-benzofuran-5-carboxylic acid | HCID 1092118 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | Methyl 2-methyl-1-benzofuran-5-carboxylate | HCID 22387841 | 81% |
Reaction Steps
5-Carboxy-2-methylbenzo[b]furan (1.9 g, 10.7 mmol) was suspended in methanol (50 ml) and concentrated sulfuric acid (0.1 ml) was added, which was followed by reflux under heating for 14 hr. After cooling, a saturated aqueous sodium hydrogencarbonate solution was added. Methanol was evaporated under reduced pressure, and the residue was extracted with methyl t-butyl ether. The organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The desiccant was filtered off and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=9/1) to give the objective compound (1.66 g, 81%) as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06348474B1 |
| Source dataset | uspto-grants-2002_02 |
| ORD ID | ord-a97596f158cd4d059a23781ac4a61349 |
| Source note | uspto-grants-2002_02 |