反应详情

温度

90 °C

Under nitrogen atmosphere, the acetic acid (1 mL) suspension of 7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one (Compound A2, 92.3 mg, 0.452 mmol) and (3,4-dichlorophenyl)hydrazine hydrochloric acid salt (Compound Y1, 96.5 mg, 0.452 mmol) was stirred at ambient temperature of 90° C. for 3.5 hr. After cooling to room temperature, the reaction mixture was added with diethyl ether and water, and the resulting mixture was extracted twice with diethyl ether. The organic layer was washed three times with water, dried over sodium sulfate, and concentrated under reduced pressure. The resulting crude product was purified by flash column chromatography {Merck Kieselgel60, solution for elution:hexane/ethyl acetate (4:1)} to obtain the title compound (pale yellow solid, 62.1 mg, 40%).

1. temperatureAfter cooling to room temperature
2. extractionthe resulting mixture was extracted twice with diethyl ether
3. washThe organic layer was washed three times with water
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe resulting crude product was purified by flash column chromatography {Merck Kieselgel60, solution for elution