反应详情

温度

60 °C

To a stirred solution of 2-methyl-3-nitro-5-(trifluoromethyl)benzoic acid (1 equiv.) in DMF (3 ml per 1 mmol), iodomethane (4 equiv.) and sodium carbonate (4 equiv.) were added. The resulting reaction mixture was stirred at 60° C. for 8 h. On completion, reaction mixture was filtered and the inorganic solid residue washed with ethyl acetate. The combined filtrate was concentrated under vacuum till dryness and the residue re-dissolved in ethyl acetate before washing with 5% sodium bicarbonate solution followed by 5M HCl solution. the organic layer was finally washed with brine, dried over sodium sulfate and concentrated to afford pure methyl 2-methyl-3-nitro-5-(trifluoromethyl)benzoate (yield 90-95%).

1. customThe resulting reaction mixture
2. customOn completion, reaction mixture
3. filtrationwas filtered
4. washthe inorganic solid residue washed with ethyl acetate
5. concentrationThe combined filtrate was concentrated under vacuum till dryness
6. dissolutionthe residue re-dissolved in ethyl acetate
7. washbefore washing with 5% sodium bicarbonate solution
8. washthe organic layer was finally washed with brine
9. dry with materialdried over sodium sulfate
10. concentrationconcentrated