Acetone → 3-Octen-2-one
反応式
[Li+].[I-].[CH3:3][C:4]([CH3:6])=[O:5].[CH:7](=O)[CH2:8][CH2:9][CH2:10][CH3:11].O>C(OCC)C>[CH3:3][C:4](=[O:5])/[CH:6]=[CH:7]/[CH2:8][CH2:9][CH2:10][CH3:11]参加物
6
実験手順
A solution of 7.73 g (58 mM) of anhydrous LiI and 1.47 ml (20 mM) of acetone in 35 ml of diethyl ether was heated to gentle reflux. To this solution was added dropwise a solution of 1.59 ml (15.0 mM) 1-pentanal in 5 ml diethyl ether over 10 minutes. The solution was then heated at reflux for 6 hours. After the solution was cooled to ambient temperature water was added and the layers separated. The ether phase was washed once with brine and dried over anhydrous MgSO4. The diethyl ether was removed by distillation at atmospheric pressure followed by distillation of the residue. There was obtained 0.52 g (27%) of a highly mobile colorless liquid. 1H NMR (CDCl3):6.80δ (dt,1H,JHH =7Hz, 16Hz), 6.01δ (d,1H,JHH =16Hz), 2.20δ (s,3H).
後処理
- temperatureThe solution was then heated
- temperatureat reflux for 6 hours
- additionwas added
- customthe layers separated
- washThe ether phase was washed once with brine
- dry with materialdried over anhydrous MgSO4
- customThe diethyl ether was removed by distillation at atmospheric pressure
- distillationfollowed by distillation of the residue
- customThere was obtained 0.52 g (27%) of a highly mobile colorless liquid
出典と根拠
- ORDレコード
- ord-4ac4febf14dd4b0893b14d6cdc31cb0a
- 出典データセット
- uspto-grants-1985_10
- 特許番号
- US04546104
反応ノート
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