HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → 2,6-Difluoroanisole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2,6-Difluorophenol | HCID 94392 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2,6-Difluoroanisole | HCID 2736897 | 81.4% |
Reaction Steps
In 254 ml of N,N-dimethylformamide was dissolved 25.4 g of 2,6-difluorophenol, followed by adding thereto 29.7 g of potassium carbonate and 83.1 g of iodomethane, and the resulting mixture was stirred at 50° C. for 2 hours. The reaction mixture was added to a mixed solvent of 200 ml of diethyl ether and 600 ml of water and the organic layer was separated. The organic layer obtained was washed with water and then a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then distilled under reduced pressure to remove the solvent. The resulting residue was purified by vacuum distillation (43-45° C./20 mmHg) to obtain 22.9 g of 2,6-difluoroanisole as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06025370 |
| Source dataset | uspto-grants-2000_02 |
| ORD ID | ord-c33f70eca4a0418e917994e853fff4dd |
| Source note | uspto-grants-2000_02 |