反应详情

A solution of 5-cyano-1-(3,4-dimethylphenyl)-4-(methylthio)-2-phenyl-6-oxo-1,6-dihydropyrimidine (3 g, 8.6 mmol) (obtained according to example 57) in chlorosulfonic acid (50.37 g, 432 mmol) was stirred at 0° C. for 2 hr and at ambient temperature for 24 hr and then poured onto ice and extracted with chloroform. The collected chloroform layer was dried over anhydrous Na2SO4 and concentrated in vacuo to yield crude compound, which was further purified by column chromatography using chloroform:methanol mixture as eluent to yield title compound (0.5 g, yield 13%). 1H-NMR (CDCl3):δ 2.37 (s, 3H), 2.65 (s, 3H), 2.68 (s, 3H), 7.26-7.55 (m, 7H). MS m/z:446.1 (M+).

1. additionpoured onto ice
2. extractionextracted with chloroform
3. dry with materialThe collected chloroform layer was dried over anhydrous Na2SO4
4. concentrationconcentrated in vacuo
5. customto yield crude compound, which
6. customwas further purified by column chromatography