関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2'-Bromoacetophenone | HCID 75060 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-Ethenyl-4,4,5,5-tetramethyl-1,3,2-dioxaborolane | HCID 5233012 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1-(2-Vinylphenyl)ethanone | HCID 220536 | 69% |
反応手順
A solution of 2′-bromoacetophenone (1.6 mL, 12 mmol), sodium hydrogencarbonate (2.5 g, 30 mmol), vinylboronic acid pinacol ester (3.0 mL, 18 mmol) and tetrakis(triphenylphosphine)palladium(0) (0.69 g, 0.60 mmol) in a mixed solvent (50 mL), which consists of water and 1,4-dioxane (1:4), was stirred at 95° C. for 2.5 hours. Water (100 mL) was added to the reaction solution and extracted with ethyl acetate (100 mL). The organic layer was washed with brine (50 mL), dried over anhydrous magnesium sulfate. After the organic layer was filtered with celite and the solvent was removed under reduced pressure, the residue was purified by silica gel column chromatography to give the title reference compound (1.2 g) as an orange oil (Yield 69%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07977371B2 |
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| 出典データセット | uspto-grants-2011_07 |
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| ORD ID | ord-2c0d823e861149d7b49a2c42d8dc5305 |
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| 出典メモ | uspto-grants-2011_07 |
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