反应详情

To a solution of (S)-4-(3,4-dichlorophenyl)-2,2-dimethyl-3,4-dihydronaphthalen-1(2H)-one (56) (0.8 g, 2.51 mmol) in CH2Cl2 (20 mL) and MeOH (15 mL)-H2O (5 mL) was added NH2OH.HCl (0.35 g, 5.04 mmol) and Et3N (1.01 g, 10.1 mmol). The resultant mixture was heated at reflux for 5 h before being concentrated. The residue was purified by silica gel column chromatography (ethyl acetate/hexane=1:7 to 1:5) to give (S,Z)-4-(3,4-dichlorophenyl)-2,2-dimethyl-3,4-dihydronaphthalen-1 (2H)-one oxime (60) (0.72 g, 84%).

1. temperatureat reflux for 5 h
2. concentrationbefore being concentrated
3. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane=1:7 to 1:5)