反应详情

To a stirred mixture of 311 mg of 4-(2-chlorophenyl)-2-phenyl-5-pyrimidinecarboxylic acid and 0.26 cc of diphenylphosphoryl azide in 5 cc of fluorobenzene was added dropwise 0.15 cc of triethylamine at room temperature. The resulting mixture was stirred at room temperature for 30 minutes and then heated at a temperature of 65°-70° C. for 10 minutes. After cooling, 0.11 cc of aniline was added and the resulting mixture was stirred heated at a temperature of 70° C. for 2 hours. After cooling, water was added to the reaction mixture and extracted with chloroform. The extract was dried over magnesium sulfate, and distilled to remove the solvent. The crude product thus obtained was purified by a silica gel column chromatography (eluent: chloroform) to obtain 200 mg of compound 7.

1. temperatureheated at a temperature of 65°-70° C. for 10 minutes
2. temperatureAfter cooling
3. stirringthe resulting mixture was stirred
4. temperatureheated at a temperature of 70° C. for 2 hours
5. temperatureAfter cooling
6. extractionextracted with chloroform
7. dry with materialThe extract was dried over magnesium sulfate
8. distillationdistilled
9. customto remove the solvent
10. customThe crude product thus obtained
11. customwas purified by a silica gel column chromatography (eluent: chloroform)