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HRID 452222作成日:2026年10月25日

Tri(butyl)vinyltin → 1-(2-Methoxy-4-nitrophenyl)-3-vinylpyridin-2(1H)-one

https://huagongshe.com/reaction/452222

反応式

関与物質

役割名称HCID仕込み量
反応物Tri(butyl)vinyltinHCID 53438229—
反応物3-Bromo-1-(2-methoxy-4-nitrophenyl)pyridin-2(1H)-oneHCID 59410145—
溶媒1,4-DioxaneHCID 31275—
生成物1-(2-Methoxy-4-nitrophenyl)-3-vinylpyridin-2(1H)-oneHCID 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

DOI10.6084/m9.figshare.5104873.v1
特許番号US08487111B2
出典データセットuspto-grants-2013_07
ORD IDord-327289a083b04419be65ffcc192100fd
出典メモuspto-grants-2013_07