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Pentenone → ethyl 4,5-dihydro-3,5-dimethyl-1H-pyrazole-1-acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pentenone | HCID 12248 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Acetic acid, 2-hydrazinyl-, ethyl ester, hydrochloride (1:1) | HCID 11593468 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | ethyl 4,5-dihydro-3,5-dimethyl-1H-pyrazole-1-acetate | HCID 67378927 | 14.1% |
反応手順
A mixture of ethyl hydrazinoacetate hydrochloride (1.55 g, 10 mmol), 3-pentene-2-one (0.95 mL, 10 mmol) and sodium bicarbonate (1.00 g, 11.9 mmol) in ethanol (10 mL) was stirred at room temperature overnight. The reaction mixture was then filtered and concentrated under reduced pressure. The resulting oil was purified by medium pressure liquid chromatography on silica gel (0 to 100% gradient of ethyl acetate in hexanes as eluant) to provide the title compound as a yellow oil (0.26 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08618137B2 |
| 出典データセット | uspto-grants-2013_12 |
| ORD ID | ord-cef1dd2f91c74bdc98647778372a4bf9 |
| 出典メモ | uspto-grants-2013_12 |