関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Chloro-2-toluidine | HCID 7251 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | Sodium hydroxide--water (1/1/1) | HCID 23719242 | — |
| 反応物 | N-(2-(2,4-dichlorophenoxy)ethyl)propylamide | HCID 86736788 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | HCID 178456755 | HCID 178456755 | 65% |
反応手順
A mixture of 19.5 g (0.075 mole) of N-(2-(2,4-dichlorophenoxy)ethyl)propylamide, 11.4 g (0.075 mole) POCl3 and 250 mls of 1,2-dichloroethane was stirred at 60° C. for six hours. The mixture was cooled to 25° C., whereupon 10.4 g (0.075 mole) of 4-chloro-2-methylaniline was added thereto. An exotherm was noted. The mixture was refluxed for 10 hours and allowed to cool. The product mixture was made basic with a 20% NaOH water solution. The product layer was separated, washed once with 200 ml of water, dried over sodium sulfate, filtered and distilled under reduced pressure to give 65% yield (based on the amide) of the desired product, a thick oil, b.p. 142° C./1.3 mm Hg . NMR confirmed the assigned structure: ##STR4##
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04183957 |
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| 出典データセット | uspto-grants-1980_01 |
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| ORD ID | ord-8a8c22dcdc1e4b128b1c1a633f1bde0f |
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| 出典メモ | uspto-grants-1980_01 |
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