関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethylamine | HCID 6341 | — |
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | 2-Chloro-N-(2-chloro-4-methyl-3-pyridinyl)-3-pyridinecarboxamide | HCID 10423868 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-(2-Chloro-4-methyl-3-pyridinyl)-2-ethylamino-3-pyridinecarboxamide | HCID 11066217 | 76.2% |
反応手順
Ethylamine (12.7 g) was added to a suspension of 21.0 g of the 2-chloro-N-(2-chloro-4-methyl-3-pyridinyl)-3-pyridinecarboxamide in 150 ml of xylene in a steel bomb. The mixture was then heated in an oil bath to 165° C. for 6 hrs. and then stirred overnight at room temperature. The solvent was removed in vacuo and water added to the residue. The product was extracted with ether, dried (sodium sulfate) and concentrated to give an oil. This was dissolved in ethyl acetate followed by hexane at which time a precipitate formed. The solid was filtered and dried to give 16.5 g of the title compound, m.p. 122°-124° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05620974 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-6931056261934f4b9e2954d3c9e52c11 |
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| 出典メモ | uspto-grants-1997_04 |
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