関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | 4-Cyclopentene-1,3-diol | HCID 278600 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Hydroxycyclopent-2-en-1-yl acetate | HCID 4428208 | 100.5% |
反応手順
0.70 gram (7.0 mmols) of 3,5-dihydroxycyclopent-1-ene and 0.83 gram (10.5 mmols) of pyridine were dissolved in 20 milliliters of anhydrous tetrahydrofuran, after which a solution of 0.70 g (9.0 mmols) of acetic acid chloride in 6 milliliters of anhydrous tetrahydrofuran was added dropwise over a period of 15 hours at room temperature in a stream of dried nitrogen, using a syringe drive. After concentrating the solvent with a rotary evaporator, 20 milliliters of ethyl acetate was added, following which the reaction mixture was washed with dilute hydrochloric acid (5 ml × 2), saturated sodium bicarbonate solution (5 ml × 2) and saturated sodium chloride solution (5 ml × 2). The organic layer was then separated and dried with anhydrous sodium sulfate. On distilling off the solvent, 1.00 gram of a colorless oil substance was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04132726 |
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| 出典データセット | uspto-grants-1979_01 |
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| ORD ID | ord-463818ef6a1e481f90874f8911e072da |
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| 出典メモ | uspto-grants-1979_01 |
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