Potassium Iodide → Methyl 2-acetylhexanoate
反応式
[CH3:1][O:2][C:3](=[O:8])/[CH:4]=[C:5](/[O-:7])\[CH3:6].[Na+].[I-].[K+].[CH2:12](Br)[CH2:13][CH2:14][CH3:15]>CN1CCCN(C)C1=O>[C:5]([CH:4]([CH2:12][CH2:13][CH2:14][CH3:15])[C:3]([O:2][CH3:1])=[O:8])(=[O:7])[CH3:6]参加物
5
反応条件
- 温度
- 80 °C
実験手順
30 g (217 mmol) of sodium (2E)-4-methoxy-4-oxo-2-buten-2-olate (Example 13A) suspended in 1,3-dimethyltetrahydro-2(1H)-pyrimidone and 1.24 g (7.5 mmol) of potassium iodide are treated dropwise with 29.8 g (217 mmol) of butyl bromide and the mixture is stirred at 80° C. for 1 h under reflux. The cooled mixture is then added to ice water and extracted with diethyl ether. The ether phase is washed with sodium thiosulphate solution, dried, concentrated and chromatographed. The eluent used is cyclohexane having an increasing ethyl acetate content.
後処理
- temperatureunder reflux
- extractionextracted with diethyl ether
- washThe ether phase is washed with sodium thiosulphate solution
- customdried
- concentrationconcentrated
- customchromatographed
出典と根拠
- ORDレコード
- ord-d000757376de4d02a6ce64ed2ce04c11
- 出典データセット
- uspto-grants-2006_02
- 特許番号
- US06998402B2
反応ノート
読み込み中…