関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Picolyl chloride | HCID 23393 | — |
| 反応物 | N'-tert-butylbenzohydrazide | HCID 299436 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | N'-t-butyl-N-benzoyl-N'-methylpyridinylhydrazine | HCID 19368177 | 20% |
反応手順
N'-t-butyl-N-benzoyl hydrazine (1.2 g), 2-chloromethyl pyridine (1.0 g) and triethylamine (2 equivalents) were stirred in dimethyl sulfoxide (15 ml) at room temperature for 2 hours. The reaction mixture was then warmed to 50° C. for 2 hours. The mixture was diluted with ether and washed with water. The organic layer was dried over magnesium sulfate, filtered and rotavapped to afford a yellow oil. The oil was chromatographed on silica gel (G:70-230 mesh) using a methylene chloride-ether mixture (1:1) as eluant to afford the purified product as a yellow gum in approximately 20% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05424333 |
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| 出典データセット | uspto-grants-1995_06 |
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| ORD ID | ord-682d8d43834e4d31a8179b4d5b542b64 |
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| 出典メモ | uspto-grants-1995_06 |
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