反应详情

温度

50 °C

A mixture of 2.5 g (11.89 mmol) 6-hydroxy-4-o-tolyl-nicotinonitrile, 3.64 g (23.78 mmol) phosphorus oxychloride in 10.0 ml dichloromethane was heated at 50° C. for 80 minutes. The mixture was cooled down to 20-25° C., poured on water by keeping the internal temperature between 20-30° C. and extracted by adding additional 80.0 ml dichloromethane. Evaporation of the organic phase in vacuo gave 2.9 g of crude product of 6-chloro-4-o-tolyl-nicotinonitrile which was purified by chromatography over silica gel (ethylacetate:hexane=4:1) to afford 2.4 g of, m.p. 112.4° C.

1. temperatureThe mixture was cooled down to 20-25° C.
2. additionpoured on water
3. custombetween 20-30° C.
4. extractionextracted
5. additionby adding additional 80.0 ml dichloromethane
6. customEvaporation of the organic phase in vacuo