化工社化工社 化学情報印刷レポート · 研究参考用
Diethyl Ether → Cyclohexanol, 1-ethynyl-, 1-acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 1-Ethynylcyclohexanol | HCID 6525 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 触媒 | Scandium(III) triflate | HCID 2734571 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Cyclohexanol, 1-ethynyl-, 1-acetate | HCID 78903 | 110.7% |
反応手順
To 3.1 g (25 mmol) 1-ethynyl-1-cyclohexanol in 25 ml acetonitrile were added 7.1 ml (75 mmol, 3 eq) acetic anhydride at −20° C. 12.3 mg (0.03 mmol) scandiumtriflate in 300 μl THF were added and the solution was stirred for 2 h. Additional 12.3 mg (0.03 mmol) scandiumtriflate in 300 μl THF were added and stirring was continued for 30 min. A saturated aqueous solution of NaHCO3 and ether were added. The layers were separated and the inorganic one was extracted with ether. The combined organic phases were washed with brine and dried over Na2SO4. Evaporation yielded 4.6 g crude 1-ethynylcyclohexyl acetate as colorless oil, MS: 166 (M).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07449483B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-a67f1e0cc08c4f6a98f30aa3663cf99f |
| 出典メモ | uspto-grants-2008_11 |