HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 19392462, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Methyl 6-hydroxy-1,4-benzodioxin-2-carboxylate | HCID 19392464 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 19392462 | HCID 19392462 | 78% |
Reaction Steps
Stir for 15 minutes at room temperature, under argon, a solution of 0.48 mmol of methyl 6-hydroxy-1,4-benzodioxin-2-carboxylate in 5 cm3 of N,N-dimethylformamide in the presence of 0.57 mmol of 60% sodium hydride suspended in oil, and then add 0.72 mmol of methyl iodide. After being stirred for 4 hours at room temperature, the reaction mixture is concentrated under reduced pressure and then extracted with methylene chloride. After the methylene chloride phases have been concentrated to dryness, the crude product is purified by chromatography on a silica column (eluant: petroleum ether/ethyl acetate, 80:20). Methyl 6-methoxy-1,4-benzodioxin-2-carboxylate is thereby obtained in a yield of 78%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05439909 |
| Source dataset | uspto-grants-1995_08 |
| ORD ID | ord-0a9aac2b18e94b91ba185454e939f3d9 |
| Source note | uspto-grants-1995_08 |