関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 2-Methyl-3-(4-methylphenyl)-2-propen-1-ol | HCID 67151049 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-(3-Chloro-2-methyl-1-propenyl)-4-methylbenzene | HCID 69150787 | 87.3% |
反応手順
To a solution of 2-methyl-3-(4-methylphenyl)-2-propen-1-ol (750 g) in toluene (2367 ml) was added dimethylformamide (29.6 ml). To the solution was added dropwise thionyl chloride (431.1 ml) at 20° C. or below and the solution was stirred at 12 to 15° C. for 1.5 hr. Water was then added thereto under ice-cooling. The toluene layer was fractionated and a 10% aqueous solution of sodium carbonate was added thereto to adjust the pH to 5. The toluene layer was fractionated again, washed successively with 5% sodium hydrogencarbonate and 5% brine. The solvent was distilled off to give the title compound as an oil (776.8 g, yield 87.3%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07420070B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-8ead58610936490782db289cb5170e76 |
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| 出典メモ | uspto-grants-2008_09 |
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