Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Potassium Iodide | HCID 4875 | — |
| Reactant | 2,3-Difluorobenzoyl chloride | HCID 519549 | — |
| Reactant | HCID 178418546 | HCID 178418546 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 83808211 | HCID 83808211 | 71.8% |
Reaction Steps
Copper(1) cyanide (6.6 g, 0.07 mol), potassium iodide (12.2 g, 0.07 mol) and xylene (70 ml) were heated at reflux for 24 h using a Dean-stark apparatus. A solution of 2,3-difluorobenzoyl chloride (10.8 g, 0.06 mol) in xylene (40 ml) was added. The resulting suspension was refluxed under N2 at 165° C. for 3 days using a Dean-Stark apparatus. After cooling, inorganic salts were removed by filtration and the filtrate concentrated in vacuo. The residue was azeotroped with toluene (2×30 ml) to give the product (7.2 g) as a brown solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08268823B2 |
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| Source dataset | uspto-grants-2012_09 |
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| ORD ID | ord-baa033e2d76a457b813fb5a2eab1b276 |
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| Source note | uspto-grants-2012_09 |
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