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Treat a 0°C solution of 4-fluorophenylacetic acid (3 g, 19.46 mmol) in H2S04 (20 mL) drop wise with nitric acid (0.913 mL, 20.44 mmol) and stir for 1 h. Pour the mixture onto ice, extract with DCM (2x), wash the combined organics with brine, dry over MgS04 and concentrate to dryness to afford the title compound (3.48 g, 90percent>). MS (ESI) m/z: 198.1 (M-H+).
74%
at 0℃; for 1 h;
At 0°C, to a solution of 2-(4-fluorophenyl)acetic acid (30 g, 0.19 mol) in cone. H2S04 (250 ml_) was added KN03 (19.6 g, 0.19 mmol) portionwise. After stirred at 0°C for 1 hr, the resulting mixture was slowly poured into ice water. The precipitated solid was filtered and dried to give the title compound (28.8 g, 74percent yield) as a yellow solid. LCMS (ESI) m/z calcd for C8H6FN04: 199.03. Found: 200.22 (M+1 )+.
59%
at 0℃; for 3.5 h;
4-fluorophenylacetic acid (6G, 38.9 MMOL) was suspended in 50 ML H2SO4 conc. And cooled to 0°C. To this suspension was added dropwise 1.75 mi HNO3 during 30 min. and then the reaction mixture was striired at 0°C for another 3h. The yellow mixture was poured into is-water and the corresponding white crystals 4-FLUOR- 3-nitrophenylacetic acid 4. 55G, 59percent was collected and dried.
A mixture of 2-(4-fluoro-3-nitrophenyl)acetic acid (28.8 g, 0.14 mmol) and cone. H2S04 (10 ml_) in MeOH (30 ml_) was stirred at 80°C overnight. The resulting mixture was quenched with ice water and extracted with EtOAc. The organic layer was washed with sat. NaHC03 aq. solution and brine, dried over Na2S04, filtered and concentrated to give the title compound (30 g, 97percent yield) as a yellow oil. LCMS (ESI) m/z calcd for C9H8FN04: 213.04. Found: 214.26 (M+1)+.
87%
for 2 h;
4-fluoro-3-nitrophenylacetic acid (4. 55g, 22.9 MMOL) was suspended in 50 ml MEOH and added 0.15 mi H2SO4 followed by reflux for 2h. After cooling the reaction mixture was poured into water and then added NAHCO3 until PH>7. The extraction with EtOAc, drying with MGS04 and evaporation in vacuo gave 5e. Yield 4. 259, 87percent.
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