HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → 1-Bromo-4-chloro-2-fluoro-3-methoxybenzene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 3-Bromo-6-chloro-2-fluorophenol | HCID 66601002 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 1-Bromo-4-chloro-2-fluoro-3-methoxybenzene | HCID 66600367 | 96.9% |
Reaction Steps
A heterogeneous mixture of 3-bromo-6-chloro-2-fluorophenol (14.4 g, 0.064 mol), methyl iodide (13.5 g, 0.096 mol) and potassium carbonate (8.8 g, 0.064 mol) in acetonitrile (100 mL) was heated under reflux for 2 hours. The mixture was cooled, diluted with water (100 mL) and extracted with ethyl ether (2×150 mL). The combined extracts were dried and concentrated. The dark oil was purified by chromatography (5% ethyl acetate in hexanes) to give 1-bromo-4-chloro-2-fluoro-3-methoxybenzene (14.8 g, 0.062 mol): 1H NMR (CDCl3): δ 7.20 (m, 1H), 7.10 (dd, 1H), 4.0 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07498468B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-9b402ece11d846a0aa5858661deb5eb4 |
| Source note | uspto-grants-2009_03 |