反应详情

温度

125 °C

A solution of 2-amino-5-(trifluoromethyl)benzoic acid (1.07 g, 5.2 mmoles) in methanol (20 ml) was treated with concentrated sulphuric acid (0.5 ml) and heated under microwave conditions at 125° C. for 2 h. The mixture was evaporated to dryness and treated with water (100 ml) then basified to saturation with potassium carbonate and extracted with ethyl acetate (2×40 ml). The combined extracts were dried over sodium sulphate, filtered and evaporated to dryness. The residue was chromatographed on silica gel eluting with an ethyl acetate/isohexane gradient. This gave the title compound 1 as a colorless oil (0.59 g, 51%).

1. customThe mixture was evaporated to dryness
2. additiontreated with water (100 ml)
3. extractionextracted with ethyl acetate (2×40 ml)
4. dry with materialThe combined extracts were dried over sodium sulphate
5. filtrationfiltered
6. customevaporated to dryness
7. customThe residue was chromatographed on silica gel eluting with an ethyl acetate/isohexane gradient