関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tributylvinyltin | HCID 81998 | — |
| 反応物 | Lithium Chloride | HCID 433294 | — |
| 反応物 | 3-Methyl-4-trifluoromethanesulfonyloxy-benzofuran-2-carboxylic acid ethyl ester | HCID 86599026 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Methyl-4-vinylbenzofuran-2-carboxylic acid ethyl ester | HCID 68713160 | 75.2% |
反応手順
To a solution of 2.48 g (7.05 mmol) of 3-methyl-4-trifluoromethanesulfonyloxy-benzofuran-2-carboxylic acid ethyl ester (Example 20, Step 2) in 30 mL of DMF was added 2.16 mL (7.40 mmol) of vinyl tributyltin, 0.898 g (21.1 mmol) of lithium chloride and 0.247 g (0.352 mmol) of tetrakis(triphenylphosphine)palladium(0). The reaction was heated to 90° C. for 3 h and then cooled to room temperature. The reaction was diluted with water and extracted with ether. The combined organics were washed with water and brine, dried over magnesium sulfate, filtered and concentrated in vacuo. The residue was chromatographed on silica gel eluting with ethyl acetate/hexanes (1:25) to provide 1.22 g of 3-methyl-4-vinylbenzofuran-2-carboxylic acid ethyl ester.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07420001B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-b0c9cf25ebb547d1903fb5e5bb5ef8a5 |
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| 出典メモ | uspto-grants-2008_09 |
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