関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Cyclohexanethiol | HCID 15290 | — |
| 反応物 | Bromopinacolone | HCID 21642 | — |
| 触媒 | Sodium tungstate | HCID 26052 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-Cyclohexylsulfonyl-3,3-dimethyl-2-butanone | HCID 22908632 | 28.7% |
反応手順
To cyclohexylthiol (23 g, 0.198 mole), a solution of potassium hydroxide (13.7 g, 0.207 mole) in ethanol (80 ml) was added dropwise at 15° C., followed by stirring at the same temperature for 24 hours. After 1-bromo-3,3-dimethyl-2-butanone (35.4 g, 0.198 mole) was added dropwise to the reaction mixture at 10°-15° C. and continued to stir at 20° C. for 5 hours, sodium tungstate (2.5 g) was added. Then, 30% hydrogen peroxide (220 g, 1.96 mole) was added dropwise at 45°-50° C. and reacted with stirring at 60°-80° C. for 30 hours. After cooling, the reaction mixture was extracted with methylene chloride (300 ml×1), the organic layer was separated, dried over anhydrous MgSO4 and evaporated to obtain 14 g of residual crude 1-cyclohexylsulfonyl-3,3-dimethyl-2-butanone as a pale yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05468589 |
|---|
| 出典データセット | uspto-grants-1995_11 |
|---|
| ORD ID | ord-5f9e35a15e6347eb878ff043c31f1985 |
|---|
| 出典メモ | uspto-grants-1995_11 |
|---|