反应详情

Methyl 2-(2-amino-4-trifluoromethylphenoxy)benzoate (11.68 g, 0.0375 mol) was mixed in tetrahydrofuran (175 ml) and sodium hydroxide (77 ml) at 40° C. for sixteen hours. The solvents were evaporated and water added to the residue. 3N hydrochloric acid was then added to the mixture until the maximum precipitate was given. The aqueous mixture was extracted with ethyl acetate (3×) and the organic phase dried over MgSO4 and evaporated. The residue was flash chromatographed (silica gel, methylene chloride/ethanol/ammonium hydroxide) to give the title compound. 1H NMR (250 MHz, CD3OD) δ7.90 (dd, 1H), 7.5 (tt, 1H), 7.2 (tt, 1H), 7.09 (d, 1H), 6.95 (dd, 1H), 6.85 (dd, 1H), 6.75 (d, 1H).

1. customThe solvents were evaporated
2. additionwater added to the residue
3. addition3N hydrochloric acid was then added to the mixture until the maximum precipitate
4. extractionThe aqueous mixture was extracted with ethyl acetate (3×)
5. dry with materialthe organic phase dried over MgSO4
6. customevaporated
7. customchromatographed (silica gel, methylene chloride/ethanol/ammonium hydroxide)