Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Acetophenonoxime | HCID 69185 | — |
| Reactant | HCID 21866628 | HCID 21866628 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86648421 | HCID 86648421 | 85.6% |
Reaction Steps
A mixture of 1-Phenyl-ethanone oxime (1.13 g), Methyl-5-(4-chloro-butyl)-2-methyl-[1,3]dioxane-2-carboxylate (prepared by processes known) (2.5 g) and cesium carbonate (4.0 g) in anhydrous dimethyl formamide was stirred at 60° C. for 18 hours in an inert atmosphere. The reaction mixture was cooled to ambient temperature, poured into ice cold water and extracted with ethyl-acetate. The combined organic extract was washed with water, brine solution, dried over sodium sulphate and evaporated under reduced pressure. Crude product was flash chromatographed over silica gel using 7% ethyl acetate in petroleum ether as eluent to obtain 2.5 g of pure product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08268867B2 |
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| Source dataset | uspto-grants-2012_09 |
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| ORD ID | ord-900d6596381c4b7795dbe2ad68332417 |
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| Source note | uspto-grants-2012_09 |
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