反应详情

0.99 g of 4-[1,1-dimethyl-3-(2-methoxyphenyl)-2-propynyloxy]benzonitrile was dissolved in 10 ml of 1,2-dichlorobenzene and heated at reflux for 1.5 hours. After cooling the solution was evaporated and the residue was chromatographed on silica gel using ethyl acetate/petroleum ether (1:4) for the elution. After recrystallization from petroleum ether (boiling point 60°-80° C.) there were obtained 480 mg of 4-(2-methoxyphenyl)-2,2-dimethyl-2H-1-benzopyran-6-carbonitrile of melting point 109°-111° C.

1. temperatureheated
2. temperatureat reflux for 1.5 hours
3. temperatureAfter cooling the solution
4. customwas evaporated
5. customthe residue was chromatographed on silica gel
6. washfor the elution
7. customAfter recrystallization from petroleum ether (boiling point 60°-80° C.) there