反应详情

A solution of isopropyl 3-(2-chloro-4-fluorophenyl)tetrahydro-5-methyl-2,4,6-trioxo-s-triazine-1(2H)-acetate (48.7 g, 0.0508 mol) in concentrated sulfuric acid is cooled to 0° C., treated with 90% nitric acid (2.6 mL), stirred at room temperature overnight, treated with 90% nitric acid (1.0 mL), stirred for 4 hours, treated with 90% nitric acid (2.0 mL), stirred at room temperature overnight, treated with 90% nitric acid (1.0 mL), stirred for 1 hour and poured onto ice. The resultant aqueous solution is filtered to obtain a solid. A solution of the solid in ether is dried over anhydrous magnesium sulfate and concentrated in vacuo to give the title product as a yellow foam which is identified by NMR spectral analyses.

1. stirringstirred for 4 hours
2. stirringstirred at room temperature overnight
3. stirringstirred for 1 hour
4. additionpoured onto ice
5. filtrationThe resultant aqueous solution is filtered
6. customto obtain a solid
7. dry with materialA solution of the solid in ether is dried over anhydrous magnesium sulfate
8. concentrationconcentrated in vacuo