反应详情

温度

40 °C

To the 2-(3-Amino-5-fluoro-2-nitro-phenyl)-malonic acid di-tert-butyl ester (140 g) in 500 mL of 4N HCl in dioxane was added 50 mL of water and heated to 40° C. for 2 days. The solution was extracted with ethyl acetate (3×'s) and the ethyl acetate washed with water (3×'s) and brine. The organic fraction was dried over MgSO4 and was concentrated to give 78 g of crude (66% pure by LC/MS); 1H NMR (500 MHz, DMSO) δ 12.40 (brs, 1H), 7.04 (s, 2H), 6.68 (dd, J=10.9 2.8 Hz, 1H), 6.47 (dd, J=10.9, 2.8 Hz, 1H), 3.80 (s, 2H).

1. extractionThe solution was extracted with ethyl acetate (3×'s) and the ethyl acetate
2. washwashed with water (3×'s) and brine
3. dry with materialThe organic fraction was dried over MgSO4
4. concentrationwas concentrated
5. customto give 78 g of crude (66% pure by LC/MS)