関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acrylate | HCID 8821 | — |
| 反応物 | Tri-o-tolylphosphine | HCID 80271 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 6-Bromo-1-benzofuran | HCID 15158722 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-(Benzofuran-6-yl)-acrylic acid ethyl ester | HCID 53971141 | — |
反応手順
A mixture of the 6-bromo-benzofuran 6-3 (1.74 g, 8.79 mmol), ethyl acrylate (1.09 g, 10.98 mmol), Pd(OAc)2 (0.099 g, 0.44 mmol), tri-o-tolylphosphine (0.268 g, 0.880 mmol), and sodium acetate (3.60 g, 43.9 mmol) in DMF (10 mL) was heated to 100° C. in a sealed tube for 4 h. The mixture was cooled to room temperature, diluted with water, and extracted with Et2O (2×40 mL). The combined organic extracts were washed with brine (30 mL), dried over MgSO4, filtered, and concentrated. The residue was purified by flash chromatography (10% ethyl acetate/hexanes) to give the ester 6-4 as an off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06297249B1 |
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| 出典データセット | uspto-grants-2001_10 |
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| ORD ID | ord-07eb08b6b1494a8dadc9edc40915f92a |
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| 出典メモ | uspto-grants-2001_10 |
|---|
