関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl Acetate | HCID 6584 | — |
| 反応物 | Benzylamine | HCID 7504 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | HCID 178426542 | HCID 178426542 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | N-Benzylacetamide | HCID 11500 | 84% |
反応手順
2.1 g. of benzylamine, 7.4 g. of methyl acetate and 1.5 g. of the sodium salt of 4,6-dimethyl-2-hydroxypyridine are dissolved in 30 ml. of dimethyl acetamide and heated at about 78° C. for 4.5 hours. As determined by thin layer chromatography, all but a trace of the benzylamine is consumed. 200 ml. of water and 0.9 ml. of concentrated hydrochloric acid are added to the reaction solution, and the solution is extracted three times with 100 ml. of ethyl acetate. The organic layer is washed with 100 ml. of water, and, after drying with sodium sulfate, concentrated and crystallized. After recrystallization from 300 ml. of ether-petroleum benzin (1:1), 2.5 of needle-like crystals of N-benzyl acetamide are obtained (yield: 84%).m.p. 60.5° - 62° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04043992 |
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| 出典データセット | uspto-grants-1977_08 |
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| ORD ID | ord-c34945f9ff3649c5a84350acbbc8f0ce |
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| 出典メモ | uspto-grants-1977_08 |
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