関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3,4,5-Trimethoxybenzaldehyde | HCID 6858 | — |
| 反応物 | (Chloromethyl)triphenylphosphonium chloride | HCID 197823 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-(2'-Chlorovinyl)-1,2,3-trimethoxy-benzene | HCID 54525441 | 72.6% |
反応手順
To a suspension of 11.94 g of (chloromethyl)-triphenylphosphonium chloride in 85 ml of absolute dimethylsulfoxide and 170 ml of absolute tetrahydrofuran were added dropwise at 0° C., while stirring in an atmosphere of dry nitrogen, 21.5 ml of n-butyllithium solution. After stirring for 30 minutes a solution of 5.48 g of 3,4,5-trimethoxybenzaldehyde in 20 ml of absolute tetrahydrofuran was added dropwise. The mixture was stirred for 30 minutes at 0° C. and then allowed to warm to room temperature. After about 4 hours the reaction mixture was worked up in the manner described in Example 5e. Column chromatography of the raw product with petroleum ether/ether (2:1) yielded 4.64 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04760087 |
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| 出典データセット | uspto-grants-1988_07 |
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| ORD ID | ord-5a2166f62c254c9180e529dcbeef73c3 |
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| 出典メモ | uspto-grants-1988_07 |
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