HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → 2'-Fluoro-6'-methoxyacetophenone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | 2-Fluoro-6-methoxybenzonitrile | HCID 523101 | — |
| Reactant | HCID 178418573 | HCID 178418573 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | 2'-Fluoro-6'-methoxyacetophenone | HCID 2737355 | — |
Reaction Steps
To a flask containing methyl magnesium bromide (1.18 g, 9.93 mmol) in ether is added dropwise 2-fluoro-6-methoxybenzonitrile (0.5 g, 3.31 mmol, Lancaster Synthesis Inc.) in benzene (9 ml). The reaction mixture is refluxed overnight. The reaction is cooled to room temperature and quenched slowly with saturated ammonium chloride (15 ml) and concentrated hydrochloric acid (1 ml). The mixture is extracted with diethyl ether (2×50 ml). The combined organic layers are dried over Na2SO4, filtered, and rotary evaporated to give 0.55 g of a crude yellow material. Purification is accomplished by vacuum column (eluting with 16% ethyl acetate in hexane). The compoundcontaining fractions are combined, yielding 5.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05399584 |
| Source dataset | uspto-grants-1995_03 |
| ORD ID | ord-484ae209999e4f22aa6abaa5b783d9fb |
| Source note | uspto-grants-1995_03 |