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Dimethylformamide → Benzyl 1,4-diazepane-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Benzyl chloroformate | HCID 10387 | — |
| 反応物 | Hexahydro-1,4-diazepine | HCID 68163 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Benzyl 1,4-diazepane-1-carboxylate | HCID 4384955 | 65.5% |
反応手順
To 230 ml of dimethylformamide were added 25 g of homopiperazine and 5.4 g of sodium bicarbonate and then 25 ml of water followed by dropwise addition of 10 g of benzyloxycarbonyl chloride with stirring under ice cooling, and the mixture was stirred at a room temperature overnight. After evaporating off dimethylformamide under a reduced pressure, the reaction mixture was extracted three times with 100 ml of chloroform, and the extract was dried over magnesium sulfate and evaporated to remove the solvent under a reduced pressure. The resulting residue was applied to a silica gel column and eluted with chloroform/methanol (9:1), to obtain 9 g of the title compound as a light yellow liquor liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05245034 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-9210acb815974a8380d54b730e8abe69 |
| 出典メモ | uspto-grants-1993_09 |