4-AMINO-2,3-DIFLUORO-5-NITRO-BENZOIC ACID

Step B: 4-Amino-2, 3-difluoro-5-nitro-benzoic acid 3 [0122] Ammonium hydroxide solution (30percent in water) (35 mL, 271 mmol) is added to a solution of 2, 3, 4-trifluoro-5-nitro-benzoic acid 2 (15 g, 67.8 mmol) in 30 mL water at 0° C. with stirring. Upon completion of ammonium hydroxide addition the reaction mixture is warmed to room temperature with stirring. After 2.5 hours, the reaction mixture is cooled to 0° C. and concentrated HCl is carefully added until pH of reaction mixture is near 0. The reaction mixture is diluted with water (30 mL) and extracted with diethyl ether (3.x.50 mL). The combined organic extracts are dried (MgSO4) and concentrated under reduced pressure to give 14 g (95percent) of pure desired product: MS APCI (-) m/z 217 (M-1) detected.Ammonium hydroxide solution (-30percent in water) (35 ml, 271 mmol) was added to a solution of 2, 3, 4-trifluoro-5- nitro-benzoic acid (15 g, 67.8 mmol) in 30 ml water at 0 Ammonium hydroxide solution (30percent in water) (35 ml, 271 mmol) is added to a solution of 2, 3, 4-trifluoro-5-nitro-benzoic acid 2 (15 g, 67.8 mmol) in 30 ml water at 0° C. with stirring. Upon completion of ammonium hydroxide addition the reaction mixture is warmed to room temperature with stirring. After 2.5 h, the reaction mixture is cooled to 0° C. and concentrated HCl is carefully added until pH of reaction mixture is near 0. The reaction mixture is diluted with water (30 ml) and extracted with diethyl ether (3.x.50 ml). The combined organic extracts are dried (MgSO4) and concentrated under reduced pressure to give 14 g (95percent) of pure desired product: MS APCI (-) m/z 217 (M-1) detected.4-Amino-2, 3-difluoro-5-nitro-benzoic acid 3Ammonium hydroxide solution (—30percent in water) (35 ml, 271 mmol) is added to asolution of 2, 3, 4-trifluoro-5-nitro-benzoic acid 2 (15 g, 67.8 mmol) in 30 ml water at 0 °C with stirring. Upon completion of ammonium hydroxide addition the reaction mixture is warmed to room temperature with stirring. After 2.5 h, the reaction mixture is cooled to 0 °C andconcentrated HC1 is carefully added until pH of reaction mixture is near 0. The reaction mixture is diluted with water (30 ml) and extracted with diethyl ether (3 x 50 ml). combined organic extracts are dried (MgSO4) and concentrated under reduced pressure to give 14 g (95percent) of pure desired product: MS APCI (-) m/z 217 (M-1) detected.Step B; 4-Amino-2.3-difluoro-5-nitrobenzoic acid; To a mixture of 2, 3, 4- trifluoro-5-nitrobenzoic acid (167.2 g, 0.756 mol, 1 equiv.) in 400 mL of distilled water was added concentrated ammonium hydroxide (28 percent NHTo a mixture of 2, 3, 4- trifluoro-5-nitrobenzoic acid (2) (167.2 g, 0.756 mol, 1 equiv) in 400 mL of distilled water EPO Solid 5-nitro-2, 3, 4-trifluorobenzoic acid (0.75 g, 0.00339 mol) was dissolved in concentrated ammonium hydroxide (25 ml) to give instantly a yellow solution. Step B

Molecular Weight:218.11
XLogP3:1.3
Hydrogen Bond Donor Count:2
Hydrogen Bond Acceptor Count:7
Rotatable Bond Count:1
Exact Mass:218.01391294
Monoisotopic Mass:218.01391294
Topological Polar Surface Area:109
Heavy Atom Count:15
Complexity:283
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes