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Hydrochloric Acid → 3-Ethynylcyclohex-2-en-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3-Ethoxycyclohex-2-ene-1-one | HCID 79216 | — |
| 反応物 | HCID 178418486 | HCID 178418486 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-Ethynylcyclohex-2-en-1-one | HCID 14570795 | — |
反応手順
To a solution of 0.5N ethynylmagnesium bromide in tetrahydrofuran (100 mL) was added under N2 and stirring 3-ethoxy-2-cyclohexen-1-one (3.75 g, 26.8 mmol) in tetrahydrofuran (12.5 mL). The mixture was stirred at RT for 20 h when it was acidified with 1N HCl (200 mL). After stirring for 15 min the acidic phase was extracted with dichloromethane (5×50 mL). The combined organic extracts were washed with water (2×50 mL) and dried (MgSO4). Evaporation of the solvent gave an oil that was purified by column chromatography (silica, ethyl acetate/hexane 1:9) to yield a yellow oil, 2.71 g, 22.6 mmol, 84%). Analysis were in agreement with literature data.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06998405B2 |
| 出典データセット | uspto-grants-2006_02 |
| ORD ID | ord-2e11234de2b24e4ea1555866d926327e |
| 出典メモ | uspto-grants-2006_02 |