有没有人合成过3？Alternative Method of Preparing methyl 3-amino-2-fluorobenzoate (Step B of Intermediate 15 Above); Step A: 2-fluoro-3-nitrobenzoic acid; Concentrated sulfuric acid (195 ml) was added carefully with stirring to a solution of 2-fluoro-3-nitrotoluene (100 g, 645 mmol) in acetic acid (1000 ml). The mixture was warmed up to 95° C. and the solution of chromium trioxide (226 g, 2.25 mol) in water (200 ml) was added dropwise with stirring over 2 h. After addition the mixture was heated with stirring for another 3 h, allowed to cool down to room temperature and poured into water (3 L). The mixture was extracted with ethyl acetate (3.x.1 L), the combined organic layers were dried over Na2SO4 and concentrated under reduced pressure to afford a light green solid, which was washed with dichloromethane (3.x.300 ml) and dried under vacuum to afford the title compound was obtained as a light yellow solid (75 g, 62.8percent). 1H NMR (300 MHz, DMSO) δ ppm 8.27 (m, 1H), 8.15 (m, 1H), 7.48 (m, 1H).查看更多
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