関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Permethric chloride | HCID 94551 | — |
| 反応物 | (2-(Difluoromethoxy)phenyl)methanol | HCID 2736992 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-Difluoromethoxybenzyl 2,2-dimethyl-3-(2',2'-dichlorovinyl)-cyclopropanecarboxylate | HCID 23317015 | 85.3% |
反応手順
6.09 g (0.035 mol) of 2-difluoromethoxybenzyl alcohol and 3.5 g (0.035 mol) of triethylamine were dissolved in 50 ml of toluene and the solution was added dropwise to a mixture of 7.95 g (0.35 mol) of 2,2-dimethyl-3-(2',2'-dichloro-vinyl)-cyclopropanecarboxylic acid chloride in 100 ml of toluene at 20°-25° C. The reaction mixture was subsequently stirred at room temperature for 3 hours and poured into 150 ml of water, the toluene phase was filtered off, washed with 100 ml of water and dried with sodium sulphate and the toluene was distilled off in vacuo. Last residues of solvent were removed by incipient distillation at a bath temperature of 60° C./0.2 to 1.0 mm Hg. 10.9 g (81% of theory) of 2-difluoromethoxybenzyl 2,2-dimethyl-3-(2',2'-dichlorovinyl)-cycIopropanecarboxylate were obtained as a viscous oil with the refractive index nD20 =1.5190.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04438275 |
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| 出典データセット | uspto-grants-1984_03 |
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| ORD ID | ord-46817ed105ab4ce6828125fc4c498f72 |
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| 出典メモ | uspto-grants-1984_03 |
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