関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | 1-Methyl-4-isopropyl-2-(3'-oxobutyl)-cyclohexan-3-one | HCID 14137252 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 14137254 | HCID 14137254 | — |
反応手順
2 g of 1-methyl-4-isopropyl-2-(3'-oxobutyl)-cyclohexan-3-one, 1.2 g of hydroxylamine hydrochloride and 100 ml of ethanol are added to a 250 ml autoclave. The autoclave is heated at 150°C for 5 hours. Thereupon, the ethanol is distilled off and the residue taken up in 40 ml of 20% potassium hydroxide solution. The mixture is extracted with diethyl ether, the extract dried over sodium sulphate and the ether subsequently distilled off. The residue is purified over a silica gel column (0.05 to 0.2 mm particles) using CHCl3 as the eluant. On distillation, there is obtained 2,5-dimethyl-8-isopropyl-5,6,7,8-tetrahydroquinoline (formula IV) with a boiling point of 70°-72°C/0.4 mm Hg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03954794 |
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| 出典データセット | uspto-grants-1976_05 |
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| ORD ID | ord-e083394cc7c44bf39deccb7efa8ca77a |
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| 出典メモ | uspto-grants-1976_05 |
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