HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → 5-(Methoxycarbonyl)thiophene-2-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 2,5-Thiophenedicarboxylic acid | HCID 20273 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 5-(Methoxycarbonyl)thiophene-2-carboxylic acid | HCID 818352 | 28% |
Reaction Steps
Thiophene-2,5-dicarboxylic acid (1.72 g, 10 mmol) and sodium carbonate (3.18 g, 30 mmol) suspended in dimethylformamide (25 mL) were stirred with methyl iodide (623 μL) at room temperature overnight. The sodium salt of the desired product was extracted with water, and 12 M hydrochloric acid was added to the combined aqueous layer. The desired product was extracted with ethyl acetate, and the combined organic layer was washed with saturated aqueous ammonium chloride, dried over anhydrous magnesium sulfate and purified by silica gel column chromatography to give 0.49 g of the desired product as a colorless solid (yield 28%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07576115B2 |
| Source dataset | uspto-grants-2009_08 |
| ORD ID | ord-8e3f014662b24a0d8ec7867874ab69c0 |
| Source note | uspto-grants-2009_08 |