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
A quantity of 3.1 gm (0.0136 mol) of N-chloroacetyl-N-(2-(3-methoxy-phenyl)-ethyl)-amine is dissolved in 270 ml of ethanol and 1530 ml of water and illuminated for ten hours under a nitrogen atmosphere with a mercury high pressure lamp at 20° to 25° C. The solution is concentrated down to about 400 ml, mixed with sodium bicarbonate, and extracted several times with ethyl acetate. The extracts are dried over magnesium sulfate and concentrated by evaporation, and the residue is purified over a silica gel column with ethyl acetate as eluant.
後処理
- concentrationThe solution is concentrated down to about 400 ml
- additionmixed with sodium bicarbonate
- extractionextracted several times with ethyl acetate
- dry with materialThe extracts are dried over magnesium sulfate
- 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-2f611ba7ad884704a1902e721b77aad1
- 出典データセット
- uspto-grants-1986_10
- 特許番号
- US04616011
反応ノート
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