関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,1,3-Trichloropropene | HCID 17378 | — |
| 反応物 | 2-Trifluoromethyl-4-(3-ethoxyphenoxy)phenol | HCID 21466192 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Sodium hydride | HCID 24758 | — |
| 生成物 | 2-Trifluoromethyl-4-(3-ethoxyphenoxy)-1-(3,3-dichloro-2-propenyloxy)benzene | HCID 21466327 | 62% |
反応手順
To a solution prepared by dissolving 0.44 g of 2-trifluoromethyl-4-(3-ethoxyphenoxy)phenol in 10 ml of N,N-dimethylfonnamide, 0.062 g of sodium hydride (60% oil-based) was added with stirring under ice cooling. After 10 minutes, a solution prepared by dissolving 0.24 g of 1,1,3-trichloro-1-propene in 5 ml of N,N-dimethylformamide was added dropwise under ice cooling. After stirring at room temperature for 10 hours, the reaction solution was poured into ice-water, and extracted twice with 50 ml of diethyl ether. Then, the ether layers were combined, washed with water, dried over anhydrous magnesium sulfate and concentrated to give a crude product. This crude product was subjected to silica gel chromatography to give 0.37 g of 2-trifluoromethyl-4-(3-ethoxyphenoxy)-1-(3,3-dichloro-2-propenyloxy)benzene, yield 62%; nD23.6 1.5369.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05530015 |
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| 出典データセット | uspto-grants-1996_06 |
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| ORD ID | ord-f65b3b2a15ee45b5af15143deb6dd724 |
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| 出典メモ | uspto-grants-1996_06 |
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