化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Carbonate → (+/-)-1-(cis-2-Phenyl-cyclohexyl)-piperidin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | (+/-)-8-(cis 2-Phenyl-cyclohexyl)-1,4-dioxa-8-aza-spiro[4,5]decane | HCID 69486512 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (+/-)-1-(cis-2-Phenyl-cyclohexyl)-piperidin-4-one | HCID 69486592 | 75.3% |
反応手順
A solution of (+/−)-8-(cis 2-phenyl-cyclohexyl)-1,4-dioxa-8-aza-spiro[4,5]decane (44.8 g) in MeOH (100 ml) and 6N HCl (445 ml) was heated to reflux for 16 h. The reaction mixture was then made basic with solid sodium carbonate, extracted with dichloromethane, dried over sodium sulphate, filtered and evaporated. The crude product was purified by flash chromatography over silica gel with n-heptane as eluent. (+/−)-1-(cis-2-phenyl-cyclohexyl)-piperidin-4-one (28.8 g, 75%) was obtained as a sticky yellow oil, MS (ISP): m/e=258.3 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07176316B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-3c13606a6f0e4b3a8fc649fc7bd67477 |
| 出典メモ | uspto-grants-2007_02 |