関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Butyl vinyl ether | HCID 8108 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | N-Methylformanilide | HCID 66737 | — |
| 反応物 | Triphosgene | HCID 94429 | — |
| 反応物 | 3-(4-Fluorophenyl)-1-(1-methylethyl)-1H-indole | HCID 736229 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-[3-(4-Fluorophenyl)-1-(1-methylethyl)-1H-indol-2-YL]-2-propenal | HCID 53395291 | 69% |
反応手順
To a solution of N-methylformanilide (30 g), butyl vinyl ether (22.2 g) in 15 ml of acetonitrile under stirring at 5° C., a solution of bis-trichloromethylcarbonate (26.1 g) in 70 ml of acetonitrile is added dropwise in 80 min. The reaction mixture is kept under stirring at 5° C. overnight, then phosphorus oxychloride (31.4 g) is added dropwise in 30 minutes, then the reaction mixture is stirred at 5° C. for 15 minutes. 3-[3-(4-Fluorophenyl)-1-(1-Methylethyl)-1H-Indole (35.8 g) and acetonitrile (25 ml) are added. The mixture is warmed to 80° C. and kept under stirring for about 24 hours. The reaction mixture is worked up as described in Example 3b to give the product (69% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091382B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-3d53efdb7a5449338c2b2634ab6dd476 |
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| 出典メモ | uspto-grants-2006_08 |
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