Reference of 863704-60-3 ,Some common heterocyclic compound, 863704-60-3, molecular formula is C12H8FNO2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.
B) 6-(4-Fluorophenyl)picolinic acid-N-oxide A mixture of picolinic acid derivative (1.0 g,, 4.6 mmol), Na2HPO4 (1.2 g) and mCPBA (1.1 g, ~70% from Aldrich) in CH2ClCH2Cl (30 mL) was stirred at rt for 2 h. Additional Na2HPO4 (0.8 g) and mCPBA (1.0 g, ~70% from Aldrich) was added to the reaction mixture and it was stirred for 3 h at rt. Another Na2HPO4 (0.5 g) and mCPBA (0.5 g, ~70% from Aldrich) was added to the reaction mixture and it was stirred at rt overnight. Next morning CHCl3 (160 mL) and 2N aq HCl (50 mL) were added to the reation mixture, the organic layer was separated, dried over MgSO4 and concentrated. The residue was purified by flash column on silica gel eluding with EtOAc/MeOH/HOAc//700:240:60 to obtain the desired product contaminated by mCPBA. This impure material was purified by preparative HPLC to obtain the desired product (175 mg, 16%) as a white solid. 1H NMR (DMF-d7) 8.45 dd, 1H, J=8.3, 2.2 Hz), 8.15 (d, 1H, J=2.2 Hz), 8.13-8.00 (mn, 4H), 7.45 (t, 2H, 8.7 Hz).
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 863704-60-3, 6-(4-Fluorophenyl)picolinic acid, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; Bristol-Myers Squibb Company; US2007/60613; (2007); A1;,
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