Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acrylonitrile | HCID 7855 | — |
| Reactant | Ethyl diphenylacetate | HCID 226748 | — |
| Reactant | Sodium ethoxide | HCID 2723922 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 67358715 | HCID 67358715 | — |
Reaction Steps
The product of Example 68A (5.58 g) was dissolved in anhydrous dioxane (15 mL). Sodium ethoxide (1.58 g) was added and the mixture was heated to 40-50° C. for 30 minutes. Acrylonitrile (1.44 mL) was added dropwise with stirring. The mixture was heated at 60-70° C. for one hour. The dioxane was removed in vacuo, and the residue was taken up in diethyl ether, washed with water and brine, dried with magnesium sulfate, filtered, and concentrated. The crude material was purified by silica gel chromatography (3-10% ethyl acetate/hexane) to obtain the title compound. MS (DCI+) m/z 311 (M+NH4)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08044069B2 |
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| Source dataset | uspto-grants-2011_10 |
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| ORD ID | ord-0750a6269058423385fff15e797184dd |
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| Source note | uspto-grants-2011_10 |
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