反応式
[CH3:1][C:2]([CH3:11])([CH2:6][CH2:7][C:8](O)=[O:9])[C:3](O)=[O:4].[NH2:12]C(N)=O>O>[CH3:1][C:2]1([CH3:11])[CH2:6][CH2:7][C:8](=[O:9])[NH:12][C:3]1=[O:4]参加物
4
反応条件
- 温度
- 160 °C
実験手順
The mixture of 10 g of 2,2-dimethylglutaric acid and 37.5 g of urea was stirred for 8 hours at 160° C. Into the reaction mixture was added water at 100° C., and the mixture was cooled to near room temperature. The mixture was extracted with ethyl acetate three times. The organic layers were washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 7.6 g of 3,3-dimethylpiperidin-2,6-dione.
後処理
- temperaturethe mixture was cooled to near room temperature
- extractionThe mixture was extracted with ethyl acetate three times
- washThe organic layers were washed with a saturated sodium chloride aqueous solution
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-8ed025b555e14d3796f947388c315afa
- 出典データセット
- uspto-grants-2012_03
- 特許番号
- US08129526B2
関連ノート
読み込み中…