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Acetate → 6-acetylamino-1-(3-methylbenzyl)-4-methylhexahydro-1H-1,4-diazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetate | HCID 175 | — |
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | m-Xylyl chloride | HCID 12102 | — |
| 反応物 | 6-acetylamino-1-methylhexahydro-1H-1,4-diazepine | HCID 15206155 | — |
| 溶媒 | Methyl Ethyl Ketone | HCID 6569 | — |
| 生成物 | 6-acetylamino-1-(3-methylbenzyl)-4-methylhexahydro-1H-1,4-diazepine | HCID 14998991 | — |
反応手順
A mixture of acetate of 6-acetylamino-1-methylhexahydro-1H-1,4-diazepine (3.0 g), 3-methylbenzyl chloride (3.5 g), potassium carbonate (17 g), sodium iodide (0.1 g) and methyl ethyl ketone (200 ml) is refluxed with stirring for 16 hours. The reaction mixture is filtered, and the filtrate is concentrated under reduced pressure. The residue is chromatographed on silica gel with elution of chloroform-methanol (20:1). Fractions containing the title compound are pooled and evaporated under reduced pressure to give the title compound as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05166341 |
| 出典データセット | uspto-grants-1992_11 |
| ORD ID | ord-ad9e5766f2a34d56ae5126485c82708d |
| 出典メモ | uspto-grants-1992_11 |