Water → 7-Methoxy-4,5-dihydro-1H-benzo[D]azepin-2(3H)-one
反応式
Cl[CH2:2][C:3]([NH:5][CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][CH3:15])[CH:9]=1)=[O:4].O>C(O)C>[CH3:15][O:14][C:10]1[CH:11]=[CH:12][C:13]2[CH2:2][C:3](=[O:4])[NH:5][CH2:6][CH2:7][C:8]=2[CH:9]=1参加物
4
実験手順
N-chloroacetyl-N-(2-(3-methoxy-phenyl)-ethyl)-amine (3.1 g, 0.0136 mol) is dissolved in ethanol (270 ml) and water (1530 ml) and illuminated for 10 hours with a high pressure mercury lamp under a nitrogen atmosphere at 20°-25° C. The solution is evaporated down (to a volume of about 400 ml), mixed with sodium bicarbonate and extracted several times with ethyl acetate. The extracts are dried over magnesium sulphate, concentrated by evaporation and the residue is purified over a silica gel column with ethyl acetate as eluant.
後処理
- customThe solution is evaporated down (to a volume of about 400 ml),
- additionmixed with sodium bicarbonate
- extractionextracted several times with ethyl acetate
- dry with materialThe extracts are dried over magnesium sulphate
- concentrationconcentrated by evaporation
- customthe residue is purified over a silica gel column with ethyl acetate as eluant
出典と根拠
- ORDレコード
- ord-73cbc105f695482ba9d70bcca9f3fa40
- 出典データセット
- uspto-grants-1988_04
- 特許番号
- US04737495
反応ノート
読み込み中…