Dimethyl Sulfate → 7-methoxy-4-methyl-3,4,5,6-tetrahydro-2H-azepine
反応式
[CH3:1][CH:2]1[CH2:8][CH2:7][NH:6][C:5](=[O:9])[CH2:4][CH2:3]1.S(OC)(O[CH3:14])(=O)=O.[OH-].[K+]>CCOCC>[CH3:14][O:9][C:5]1[CH2:4][CH2:3][CH:2]([CH3:1])[CH2:8][CH2:7][N:6]=1参加物
5
反応条件
- 温度
- 120 °C
実験手順
A mixture of 5-methylazepan-2-one (1.6 g) and dimethyl sulfate (2 g, 15.9 mmol) was stirred at 120° C. for 4 h. After it was cooled to room temperature, the reaction mixture was diluted with 10 mL ether and adjusted to pH 6 with aqueous KOH. The mixture was extracted with ether (2×50 mL). The organic layer was washed with brine and dried over anhydrous sodium sulfate. After filtration and concentration, the crude (E)-7-methoxy-4-methyl-3,4,5,6-tetrahydro-2H-azepine (1.2 g) was used for the next step without further purification.
後処理
- temperatureAfter it was cooled to room temperature
- extractionThe mixture was extracted with ether (2×50 mL)
- washThe organic layer was washed with brine
- dry with materialdried over anhydrous sodium sulfate
- filtrationAfter filtration and concentration
- customthe crude (E)-7-methoxy-4-methyl-3,4,5,6-tetrahydro-2H-azepine (1.2 g) was used for the next step without further purification
出典と根拠
- ORDレコード
- ord-029b309ad3bd41ef956191c8de2b65ab
- 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…