関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 2-Cyclohexen-1-OL | HCID 13198 | — |
| 生成物 | 3-Acetoxycyclohexene | HCID 11116148 | 94% |
反応手順
To a solution of 2-cyclohexen-1-ol (16) (45.5 mmol, 5.02 mL) in pyridine (0.27 mol, 22 mL) at 0° C., acetic anhydride was added dropwise and the reaction mixture was stirred at 0° C. for ½ h. The ice bath was removed, and the mixture was stirred at room temperature overnight. The mixture was diluted with EtOAc, washed with HCl (1 N), saturated NaHCO3, brine, and concentrated in vacuo to give 6 g (94%) of the crude product 17 which was used in the next step without further purification. TLC with 20% EtOAc/Hexane, stained with 5% H2SO4/EtOH, Rf for (16): 0.4, Rf for (17): 0.8.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08889719B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-9b69b1c899954ecc88c475798102edee |
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| 出典メモ | uspto-grants-2014_11 |
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