反応式
Cl.Cl[CH2:3][CH2:4][CH:5]1[CH2:11][N:10]([CH3:12])[C:9](=[O:13])[C:8]2[CH:14]=[CH:15][CH:16]=[N:17][C:7]=2[O:6]1.[CH3:18][NH:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>>[CH3:12][N:10]1[C:9](=[O:13])[C:8]2[CH:14]=[CH:15][CH:16]=[N:17][C:7]=2[O:6][CH:5]([CH2:4][CH2:3][N:19]([CH3:18])[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH2:11]1参加物
反応条件
- 温度
- 95 °C
実験手順
2-(2-Chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepin-5(4H)-one hydrochloride, 4.00 g (0.015 mole) was dissolved in N-methylaniline (30 ml) and heated to 95° C. with stirring for 2 days. Excess N-methylaniline was removed by rotary evaporation (95° C., vacuum pump). The residue was taken up in chloroform (80 ml) and washed with dilute aqueous sodium hydroxide (30 ml). The chloroform layer was decolorized with activated carbon and dried over sodium sulfate, filtered and concentrated by rotary evaporation. The remaining residue was dissolved in ethyl acetate (50 ml) and purified by high pressure liquid chromatography using a silica gel column and ethyl acetate as the eluent. After purification, crystals formed from ethyl acetate. These crystals were recrystallized from ethyl acetate, giving 1.40 g (31%) of pale brown crystals.
後処理
- customExcess N-methylaniline was removed by rotary evaporation (95° C., vacuum pump)
- washwashed with dilute aqueous sodium hydroxide (30 ml)
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated by rotary evaporation
- dissolutionThe remaining residue was dissolved in ethyl acetate (50 ml)
- custompurified by high pressure liquid chromatography
- customAfter purification, crystals
- customformed from ethyl acetate
- customThese crystals were recrystallized from ethyl acetate
出典と根拠
- ORDレコード
- ord-78147b45cdc7467d8d67941c2d646da8
- 出典データセット
- uspto-grants-1988_02
- 特許番号
- US04727152
関連ノート
読み込み中…