関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-(4-Chlorophenyl)ethylamine | HCID 97803 | — |
| 反応物 | 1,2,2-Trichloro-3,3-dimethylcyclopropanecarboxylic acid chloride | HCID 13654698 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N-(4-chloro-alpha-methylbenzyl)-1,2,2-trichloro-3,3-dimethylcyclopropanecarboxamide | HCID 13654700 | 90.1% |
反応手順
4-Chloro-α-methylbenzylamine (15.6 g) and triethylamine (10.1 g) were dissolved in toluene (150 ml). With stirring, a solution of 1,2,2-trichloro-3,3-dimethylcyclopropanecarboxylic acid chloride (23.6 g) in toluene (30 ml) was added dropwise to the solution at 0° to 10° C. After the addition, the mixture was stirred at room temperature for 2 hours. The reaction mixture was poured into ice water, and the aqueous layer was extracted with toluene. The toluene layers were combined, washed with a 1% aqueous solution of hydrochloric acid, a 1% aqueous solution of sodium hydroxide and water in this order, and then dried over anhydrous sodium sulfate. Toluene was evaporated under reduced pressure to give the desired N-(4-chloro-α-methylbenzyl)-1,2,2-trichloro-3,3-dimethylcyclopropanecarboxamide (32 g) represented by the following formula as colorless crystals. mp. 138°-139° C. ##STR35##
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05061731 |
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| 出典データセット | uspto-grants-1991_10 |
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| ORD ID | ord-4f36cc5acd4d49c18baee724834229e6 |
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| 出典メモ | uspto-grants-1991_10 |
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