Dimethyl Carbonate → Methyl 4,4-dimethyl-2-oxocyclohexane-1-carboxylate
反応式
[CH3:1][C:2]1([CH3:9])[CH2:7][CH2:6][CH2:5][C:4](=[O:8])[CH2:3]1.[H-].[Na+].[C:12](=O)([O:15]C)[O:13][CH3:14]>C1(C)C=CC=CC=1>[CH3:1][C:2]1([CH3:9])[CH2:7][CH2:6][CH:5]([C:12]([O:13][CH3:14])=[O:15])[C:4](=[O:8])[CH2:3]1参加物
5
実験手順
A solution of 3,3-dimethylcyclohexanone (0.5 g, 3.97 mmol, 1 equiv) and sodium hydride in toluene was stirred at rt for half an hour. To the mixture was added dimethyl carbonate and heated at reflux for 5 h. After the reaction was cooled to rt, the reaction mixture was quenched with water and extracted with ethyl acetate (3×50 mL). The combined organic layers were washed with brine and dried over anhydrous sodium sulfate, then concentrated under reduced pressure to give the crude product, which was directly used for the next step.
後処理
- temperatureheated
- temperatureat reflux for 5 h
- customthe reaction mixture was quenched with water
- extractionextracted with ethyl acetate (3×50 mL)
- washThe combined organic layers were washed with brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-0d546ada348d4a088d8cbc1313ab3dab
- 出典データセット
- uspto-grants-2014_07
- 特許番号
- US08772301B2
反応ノート
読み込み中…