関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Cyclopropanecarbonyl chloride | HCID 77637 | — |
| 反応物 | 2-[2-Chloro-4-(3,5-difluorophenoxy)phenoxy]ethylamine | HCID 15766489 | — |
| 生成物 | N-{2-[2-chloro-4-(3,5-difluorophenoxy)phenoxy]ethyl}-cyclopropane carboxyamide | HCID 131718735 | — |
反応手順
To a mixture of 200 g (0.667 mol) of 2-[2-chloro-4-(3,5-difluorophenoxy)phenoxy]ethylamine, 81 g (0.80 mol) of triethylamine and 8 liter of toluene, there was added dropwise a solution of 70 g (0.67 mol) of cyclopropane carbonylchloride in 2 liter of toluene with stirring at a temperature of from 5° C. to 10° C. After 2 hours, the reaction mixture was stirred at a room temperature for 15 hours. After the reaction was completed, the resultant mixture was washed twice with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography to give 163 g of N-{2-[2-chloro-4-(3,5-difluorophenoxy)phenoxy]ethyl}-cyclopropane carboxyamide as a white crystal (m.p. 89°-90° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05364966 |
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| 出典データセット | uspto-grants-1994_11 |
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| ORD ID | ord-501cf6192595489a813150590a207aaf |
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| 出典メモ | uspto-grants-1994_11 |
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