Water → 1-(2-Methoxyethyl)-6-phenylazepan-2-one
反応式
[H-].[Na+].[C:3]1([CH:9]2[CH2:15][NH:14][C:13](=[O:16])[CH2:12][CH2:11][CH2:10]2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH3:17][O:18][CH2:19][CH2:20]Br.O>CN(C)C=O>[CH3:17][O:18][CH2:19][CH2:20][N:14]1[CH2:15][CH:9]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:10][CH2:11][CH2:12][C:13]1=[O:16]参加物
6
実験手順
Sodium hydride (60% dispersion in mineral oil; 0.32 g, 8.03 mmol) was added to a solution of 6-phenylazepan-2-one (0.76 g, 4.02 mmol) in N,N-dimethylformamide (15 mL) at 0° C., followed by the addition of 2-bromoethyl methyl ether (0.837 g, 6.03 mmol), and the mixture was allowed to warm to ambient temperature. After 21 h, water was added and the mixture was extracted with ethyl acetate (3×). The combined organic extracts were washed with water (3×), saturated brine, dried over sodium sulfate, filtered and concentrated. MS 248 (M+1).
後処理
- extractionthe mixture was extracted with ethyl acetate (3×)
- washThe combined organic extracts were washed with water (3×), saturated brine
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-106b07842c15456696a88737fcf93222
- 出典データセット
- uspto-grants-2009_05
- 特許番号
- US07534784B2
反応ノート
読み込み中…