反応式
[CH2:1]([CH:3]1[CH2:8][CH2:7][CH2:6][CH2:5][C:4]1=[N:9]O)[CH3:2].[Na].Cl>C(O)C.O>[CH2:1]([CH:3]1[CH2:8][CH2:7][CH2:6][CH2:5][CH:4]1[NH2:9])[CH3:2]参加物
6
反応条件
- 温度
- 110 °C
実験手順
To the solution of 2-ethyl-1-(hydroxyimino)cyclohexane (6.8 g, 48.5 mmol) in ethanol (75 mL) were added sodium pieces (about 8.0 g) in portions, and the reaction was heated to reflux at 110° C. overnight. More sodium pieces were added, and the reaction was stirred for another 6 hours. The reaction was treated with concentrated HCl (12 M, 4.0 mL) in water (25 mL). Ethanol was removed in vacuo. The aqueous layer was washed with ether (10 mL), and treated with aqueous KOH (25 mL) and extracted with ether (3×20 mL). The combined organic extracts were washed with brine (20 mL), dried over sodium sulfate, and concentrated in vacuo to give 2-ethylcyclohexylamine as an off-white oil.
後処理
- temperaturethe reaction was heated
- customEthanol was removed in vacuo
- washThe aqueous layer was washed with ether (10 mL)
- additiontreated with aqueous KOH (25 mL)
- extractionextracted with ether (3×20 mL)
- washThe combined organic extracts were washed with brine (20 mL)
- dry with materialdried over sodium sulfate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-9ba08e3aa54d44e0b001e09a709cd3cf
- 出典データセット
- uspto-grants-2006_02
- 特許番号
- US06995269B2
関連ノート
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