Dimedone → 2-Cyclohexen-1-one, 3-methoxy-5,5-dimethyl-
反応式
[CH3:1][C:2]1([CH3:10])[CH2:7][C:6](=[O:8])[CH2:5][C:4](=[O:9])[CH2:3]1.[C:11]([O-])(O)=O.[Na+]>CO.ClCCl.[Cl-].[Ti+4].[Cl-].[Cl-].[Cl-]>[CH3:11][O:8][C:6]1[CH2:7][C:2]([CH3:10])([CH3:1])[CH2:3][C:4](=[O:9])[CH:5]=1参加物
6
実験手順
A solution of 5,5-dimethyl-cyclohexane-1,3-dione (80.0 g, 0.57 mol) in anhydrous methanol (600 mL) was treated with a 1M solution of titanium chloride (TiCl4) in dichloromethane (17.2 mL). After stirring 1 hour at room temperature, the mixture was slowly poured into cold 5% NaHCO3 solution and extracted with diethyl ether (450 mL×6). The organic layers were collected, washed with brine, dried on Na2SO4 and evaporated to dryness affording the title compound (81.5 g, 92% yield) as a pale yellow oil.
後処理
- extractionextracted with diethyl ether (450 mL×6)
- customThe organic layers were collected
- washwashed with brine
- customdried on Na2SO4
- customevaporated to dryness
出典と根拠
- ORDレコード
- ord-bfd5b4a57af1495d89005a7d29524131
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08541429B2
反応ノート
読み込み中…