反应详情

The mixture of 6-methyl-4-(3-nitrophenyl)-2-phenyl-5-pyrimidinecarboxylic acid (5 g), triethylamine (1.5 g) and diphenylphosphoyrylazide (4.1 g) in benzene was refluxed for 2 hours and 2-dimethylaminoethylamine (1.6 g) was added. After continuing the reflux for 2 hours, the reaction mixture was poured into a mixture of Diethylether (100 ml) and saturated sodium hydrogen carbonate (50 ml). The separated organic layer was dried over magnesium sulfate and evaporated in vacuo. The residual substance was column-chromatographed on alumina. The eluted active fraction with chloroform was concentrated in vacuo and added 0.1 mole hydrochloric acid in isopropyl ether. The resulted crystalline was collected and washed with diethyl ether, dried to give 5-[3-(2-dimethylaminoethyl)ureido]-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine hydrochloride (0.98 g).

1. temperaturewas refluxed for 2 hours
2. temperaturereflux for 2 hours
3. dry with materialThe separated organic layer was dried over magnesium sulfate
4. customevaporated in vacuo
5. customThe residual substance was column-chromatographed on alumina
6. concentrationThe eluted active fraction with chloroform was concentrated in vacuo
7. customThe resulted crystalline was collected
8. washwashed with diethyl ether
9. customdried