Water → 7-Methoxy-4,5-dihydro-1H-benzo[D]azepin-2(3H)-one
반응식
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]=1참가 물질
4
실험 절차
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 in a nitrogen atmosphere at 20°-25° C. with a high pressure mercury lamp. The solution is evaporated down (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. Yield: 820 mg. Mp: 152°-154° C.
후처리
- customThe solution is evaporated down (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
출처 및 근거
- ORD 기록
- ord-be8095c5a2534eaaaaeeb846fad92dff
- 출처 데이터셋
- uspto-grants-1986_04
- 특허 번호
- US04584293
반응 노트
불러오는 중…