Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 22929815 | HCID 22929815 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Dibromine monoxide | HCID 14513628 | — |
| Product | HCID 22929663 | HCID 22929663 | — |
Reaction Steps
After dissolving 1-[3-amino-5-(tert-butyl)-4-methoxyphenyl]-1-ethanone (180 g) in dimethylformamide (800 ml), dibromoether (125 ml), potassium carbonate (225 g) and sodium iodide (12.2 g) were added and the mixture was stirred at 80° C. for 48 hours. The reaction mixture was cooled to room temperature, 3 l of ether was added and the mixture was washed 3 times with water. The organic layer was dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to yield the title compound (76 g) as yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07244730B2 |
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| Source dataset | uspto-grants-2007_07 |
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| ORD ID | ord-b0da6e4a1ba24b8c9cd8bd4cc4bb124f |
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| Source note | uspto-grants-2007_07 |
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