関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 反応物 | 2-Butyl-3,5,5-trimethyl-2-cyclohexen-1-one | HCID 4100747 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | 4-(Dibutylamino)-2-methoxybenzaldehyde | HCID 14643903 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-[2-(4-Dibutylamino-2-methoxyphenyl)vinyl]-2-butyl-5,5-dimethyl-2-cyclohexenone | HCID 68009322 | 10.6% |
反応手順
0.3 g (13.0 mmol) of sodium was dissolved in 15 ml of ethanol. Next, 2.63 g (10.0 mmol) of 4-dibutylamino-2-methoxybenzaldehyde and 2.22 g (11.0 mmol) of 2-butyl-3,5,5-trimethyl-2-cyclohexenone were dissolved in 5 ml of ethanol and added to the mixture. To this mixture, 0.36 g of ammonium acetate was added and the mixture was stirred with heating at 60° C. for 22 hours. To the mixture, 100 ml of ethyl acetate was added. Washing with a saturated saline solution, drying over anhydrous sodium sulfate, and concentration were performed. The residual liquid was purified by silica gel column chromatography to give 465 mg of a dark red oily matter (yield: 10.6%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846955B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-3c4daaf907ac4998a292cf2de3c55ec4 |
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| 出典メモ | uspto-grants-2014_09 |
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