関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl trichloroacetate | HCID 10588 | — |
| 反応物 | 4-(4-Aminophenoxy)-N-methylpicolinamide | HCID 16655129 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N-methyl-4-(4-(2,2,2-trichloroacetamido)phenoxy)picolinamide | HCID 68728447 | 87.6% |
反応手順
4-(4-aminophenoxy)-N-methylpicolinamide (35 g, 0.144 mol) was mixed with ethyl-2,2,2-trichloroacetate (50 ml, 0.27 mol) in toluene (350 ml) at ambient temperature. The mixture was then heated to 100° C. under distillation mode for 2-3 hours. The organic solvent was degassed under reduced pressure to obtain oil. This oil was triturated with hexane (500 ml) to obtain (49 g) of the desired solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08445687B2 |
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| 出典データセット | uspto-grants-2013_05 |
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| ORD ID | ord-284905d4c53f4ad3bcd9f9c896f6b010 |
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| 出典メモ | uspto-grants-2013_05 |
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