反应详情

A mixture of 5.29 g of 6-chloro-2-benzyloxy-3-nitropyridine, 6.77 g of 2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenol, 3.32 g of potassium carbonate and 30 ml of N,N-dimethylformamide was stirred for 30 minutes at room temperature, then at 50° C. for 2.5 hours. The resulted residue was added to ice water, extracted with ethyl acetate, and organic layer was washed with saturated saline, dried over anhydrous magnesium sulfate, and concentrated. The residue was recrystallized from ethyl acetate and hexane to obtain 9.11 g of 6-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-benzyloxy-3-nitropyridine.

1. waitat 50° C. for 2.5 hours
2. extractionextracted with ethyl acetate, and organic layer
3. washwas washed with saturated saline
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated
6. customThe residue was recrystallized from ethyl acetate and hexane