Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Potassium Iodide | HCID 4875 | — |
| Reactant | Potassium Acetate | HCID 517044 | — |
| Reactant | HCID 22227643 | HCID 22227643 | — |
| Solvent | Acetic Anhydride | HCID 7918 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 22227642 | HCID 22227642 | 66.3% |
Reaction Steps
A solution of 20.6 g potassium acetate and 3.49 g potassium iodide in 306 ml acetic anhydride was stirred and the product (VII) of Ex. 1 added. The reaction mixture was refluxed with stirring for 12-16 hrs, then cooled to 25° C. and diluted with 100 ml EtOAc. The reaction mixture was filtered, and the filtrate concentrated in vacuo. Ethyl acetate (400 ml) was added and the resultant solution was washed with 2×200 ml of 50% aq. NaHCl3. The organic layer was isolated, dried (MgSO4 an.), filtered and concentrated in vacuo. Purification by flash chromatography yielded product (VIII) in 66.3% yield as a viscous light yellow oil (93% pure).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08778301B2 |
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| Source dataset | uspto-grants-2014_07 |
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| ORD ID | ord-7c4f290d45ca42d29228c12d555a4566 |
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| Source note | uspto-grants-2014_07 |
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