化工社化工社 化学情報印刷レポート · 研究参考用
Hydrazine hydrate (1:1) → HCID 178423887、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | 2-[(Dimethylamino)methylene]-5,5-dimethylcyclopentanone | HCID 69583590 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 178423887 | HCID 178423887 | 102.8% |
反応手順
To a solution of 2-[(dimethylamino)methylene]-5,5-dimethylcyclopentanone (12.5 g, 75 mmol) in ethanol (100 mL) at room temperature was added hydrazine hydrate (4 mL, 82.3 mmol). The reaction mixture was heated at reflux overnight. It was then cooled to room temperature and concentrated. Water (700 mL) was added to the residue, and the resulting solution was extracted twice with diethyl ether (2×250 mL). The organic extracts were combined, dried over MgSO4 and concentrated to give the title compound as an oil (10.5 g). 1H NMR indicated the oil to be ˜60% pure. It was used directly for Step C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07138361B2 |
| 出典データセット | uspto-grants-2006_11 |
| ORD ID | ord-f657392d3ec74be3a5f9a13e2dda1db6 |
| 出典メモ | uspto-grants-2006_11 |