反应详情

温度

165 °C

A mixture of 4.0 g (20 mmol) of 1,4-dihydro-7-methoxy-4-oxo-quinoline-3-carbonitrile and 8.3 g (40 mmol) of phosphorous pentachloride was heated at 165° C. for 3 hours. The mixture was diluted with hexanes and the solid was collected. The solid was mixed with brine and dilute sodium hydroxide solution and extracted several times with a mixture of tetrahydrofuran and ethyl acetate. The solution was dried over magnesium sulfate and filtered through a pad of silica gel giving 3.7 g of 4-chloro-7-methoxy-quinoline-3-carbonitrile as a white solid: mass spectrum (electrospray, m/e): M+H 218.9.

1. customthe solid was collected
2. additionThe solid was mixed with brine and dilute sodium hydroxide solution
3. extractionextracted several times
4. additionwith a mixture of tetrahydrofuran and ethyl acetate
5. dry with materialThe solution was dried over magnesium sulfate
6. filtrationfiltered through a pad of silica gel giving 3.7 g of 4-chloro-7-methoxy-quinoline-3-carbonitrile as a white solid