Lithium → 2-Nonenal
反応式
[C:1](Cl)(=[O:10])/[CH:2]=[CH:3]/[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9].[Li]>COCCOCCOC>[CH:1](=[O:10])/[CH:2]=[CH:3]/[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9]参加物
4
反応条件
- 温度
- -78 °C
実験手順
Trans-2-nonenoyl chloride (170 g, 1 mole) is dissolved in 500 ml of diglyme and placed in a flask fitted with a mechanical stirrer, dripping funnel, low temperature thermometer and nitrogen inlet and outlet. The flask is flushed with nitrogen and cooled to -78°C in a dry ice acetone bath. To the flask, lithium tri-t-butoxyaluminohydried (254 g, 1 mole) in 1000 ml of diglyme is added over a period of 7 hours. The cooling bath is removed and the contents of the flask are allowed to warm to room temperature. The contents are poured onto crushed ice and the oily layer taken up in ether. The ether solution is dried over sodium sulfate, concentrated and vacuum distilled to give trans-2-nonenal.
後処理
- customplaced in a flask
- customfitted with a mechanical stirrer
- customThe flask is flushed with nitrogen
- customThe cooling bath is removed
- temperatureto warm to room temperature
- additionThe contents are poured
- customonto crushed ice
- dry with materialThe ether solution is dried over sodium sulfate
- concentrationconcentrated
- distillationvacuum distilled
出典と根拠
- ORDレコード
- ord-444a83e2455c49cbb22f985f85b6fe9b
- 出典データセット
- uspto-grants-1976_06
- 特許番号
- US03962321
反応ノート
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