化工社化工社 化学情報印刷レポート · 研究参考用
Dimedone → 2-Cyclohexen-1-one, 3-methoxy-5,5-dimethyl-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimedone | HCID 31358 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 触媒 | Diamminetetrachlorotitanate(IV) | HCID 160960 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Cyclohexen-1-one, 3-methoxy-5,5-dimethyl- | HCID 138318 | 92% |
反応手順
A solution of 5,5-dimethyl-cyclohexane-1,3-dione (80.0 g, 0.57 mol) in anhydrous methanol (600 mL) was treated with a 1M solution of titanium chloride (TiCl4) in dichloromethane (17.2 mL). After stirring 1 hour at room temperature, the mixture was slowly poured into cold 5% NaHCO3 solution and extracted with diethyl ether (450 mL×6). The organic layers were collected, washed with brine, dried on Na2SO4 and evaporated to dryness affording the title compound (81.5 g, 92% yield) as a pale yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541429B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-bfd5b4a57af1495d89005a7d29524131 |
| 出典メモ | uspto-grants-2013_09 |