Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 3-Fluoroanisole | HCID 9975 | — |
| Reactant | 4-Fluorobenzoyl chloride | HCID 67879 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Solvent | Nitrobenzene | HCID 7416 | — |
| Product | HCID 22475212 | HCID 22475212 | 25% |
Reaction Steps
To a cold (5° C.) mixture of aluminium trichloride (144 g, 1.08 mol, 1.13 eq.) in nitrobenzene (450 mL) was slowly added a solution of 4-fluorobenzoyl chloride (120 mL, 1 mol, 1.05 eq.) in nitrobenzene (200 mL). 3-fluoroanisole (108.5 mL, 0.95 mol) was slowly added to the reaction mixture. The cooling bath was removed and the reaction mixture was stirred 3 h at 20° C., and poured into ice-water. The aqueous layer was extracted with dichloromethane (2 times). The combined organic layers were dried over sodium sulfate, filtered and the volatiles were removed in vacuo. The crude mixture was crystallized in cyclohexane, filtered and the solid was washed with cyclohexane. The solid was dried in vacuo, affording the title compound (57.78 g, 25%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06900227B2 |
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| Source dataset | uspto-grants-2005_05 |
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| ORD ID | ord-14067e2b01164c33ad04c0cc766f62c7 |
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| Source note | uspto-grants-2005_05 |
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