関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-chloro-N-(2,4,6-trichlorophenyl)acetamide | HCID 31122 | — |
| 反応物 | N-Methylpiperazine-2-carboxamide | HCID 14722545 | — |
| 溶媒 | 2-Methoxyethanol | HCID 8019 | — |
| 生成物 | 3-((methylamino)carbonyl)-N-(2,4,6-trichlorophenyl)-1-piperazineacetamide | HCID 14722546 | 24.4% |
反応手順
A mixture of 15.33 parts of N-methyl-2-piperazinecarboxamide, 27.2 parts of 2-chloro-N-(2,4,6-trichlorophenyl)acetamide, 9.8 parts of N,N-diethylethanamine and 300 parts of 2-methoxyethanol was stirred for 3 hours at 60° C. The reaction mixture was evaporated. The residue was taken up in a small amount of water and treated with sodium carbonate. The product was extracted three times with dichloromethane. The combined extracts were dried, filtered and evaporated. The residue was crystallized from acetonitrile. The product was filtered off (the filtrate was set aside) and dried, yielding a first fraction of 9.27 parts (24.4%) of 3-((methylamino)carbonyl)-N-(2,4,6-trichlorophenyl)-1-piperazineacetamide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04968684 |
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| 出典データセット | uspto-grants-1990_11 |
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| ORD ID | ord-a48e90cd4289448397265026f8de01c7 |
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| 出典メモ | uspto-grants-1990_11 |
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