Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Acetamide | HCID 178 | — |
| Edukt | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Edukt | Methyl 2-Chloro-6-methylisonicotinate | HCID 2759833 | — |
| Katalysator | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| Katalysator | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | HCID 67510177 | HCID 67510177 | 89% |
Reaktionsschritte
A mixture of methyl 2-chloro-6-methylisonicotinate (2.00 g, 10.8 mmol), acetamide (1.27 g, 21.6 mmol), tris(dibenzylideneacetone)dipalladium(0) (0.20 g, 0.22 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (0.37 g, 0.65 mmol), tripotassium phosphate (2.74 g, 12.9 mmol) and 1,4-dioxane (26 mL) is heated by microwave irradiation at 150° C. for 1 hr. After cooling to room temperature, the mixture is filtered through a pad of celite. The filtrate is concentrated under reduced pressure and the residue is purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (4:11:3) to give 1.99 g (89% yield) of the title compound as a yellow solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US09302991B2 |
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| Quelldatensatz | uspto-grants-2016_04 |
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| ORD ID | ord-59773bcf0634409fb3d5a05fc39d70fe |
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| Quellennotiz | uspto-grants-2016_04 |
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