反应详情

18 mg of Isoamyl nitrite was added to a mixture of 0.16 g of 3-{2-amino-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-{1-(methoxycarbonyl)ethoxy}pyridine, 63 mg of copper(I) chloride, 129 mg of copper(II) chloride and 1.5 ml acetonitrile dropwise at 0° C. and the mixture was stirred for 10 minutes, then at room temperature for 1 hour. This reaction solution was poured into a mixture of 1N hydrochloric acid and ice, and extracted with ethyl acetate. The organic layer was washed with saturated saline, dried over anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.12 g of 3-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}-2-{1-(methoxycarbonyl) ethoxy} pyridine (as a mixture of two diastereomerical isomers) [present compound 7-2].

1. waitat room temperature for 1 hour
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with saturated saline
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated