関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tri(butyl)vinyltin | HCID 53438229 | — |
| 反応物 | 3-Bromo-1-(2-methoxy-4-nitrophenyl)pyridin-2(1H)-one | HCID 59410145 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1-(2-Methoxy-4-nitrophenyl)-3-vinylpyridin-2(1H)-one | HCID 59410176 | — |
反応手順
100 g (308 mmol) of the compound from Example 28A are dissolved in 1.4 l of anhydrous dioxane, and 8.9 g (7.7 mmol) of tetrakis(triphenylphospine)palladium and 117 g (370 mmol) of tributylvinyltin are added. The mixture is heated at reflux for 16 h. The reaction solution is then allowed to cool and filtered through kieselguhr. The filtrates are concentrated to dryness under reduced pressure. The residue is chromatographed on silica gel using a gradient of cyclohexane and ethyl acetate. The product-containing fractions are combined and concentrated to dryness under reduced pressure. Petroleum ether is added until crystallization sets in. The crystals are filtered off and dried under reduced pressure. This gives 37 g (41% of theory) of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08487111B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-327289a083b04419be65ffcc192100fd |
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| 出典メモ | uspto-grants-2013_07 |
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