反应详情

To a mixture of sodium hydride (122 mg, 3.04 mmol) in 6 mL of dimethylsulfoxide is added benzyl alcohol (91 mg, 0.84 mmol). The solution is stirred at room temperature for 40 minutes. 4-[(2,4-Dichloro-5-methoxyphenyl)amino]-7-fluoro-6-methoxy-3-quinolinecarbonitrile (300 mg, 0.76 mmol) is added and the reaction mixture is heated at 100° C. for 3 hours then cooled to room temperature and allowed to stir overnight. The reaction mixture is poured into saturated sodium bicarbonate and the solids are collected by filtration. Purification by flash column chromatography eluting with 10% ethyl acetate in dichloromethane provides 267 mg of 7-benzyloxy-4-[(2,4-dichloro-5-methoxyphenyl)amino]-6-methoxy-3-quinolinecarbonitrile, mp 198-200° C.

1. temperaturethe reaction mixture is heated at 100° C. for 3 hours
2. temperaturethen cooled to room temperature
3. stirringto stir overnight
4. filtrationthe solids are collected by filtration
5. customPurification by flash column chromatography
6. washeluting with 10% ethyl acetate in dichloromethane