With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.903522-29-2, name is 3,5-Difluoroisonicotinic acid, molecular formula is C6H3F2NO2, molecular weight is 159.09, as common compound, the synthetic route is as follows.Recommanded Product: 903522-29-2
General procedure: DMF (10 mg, 0.137 mmol) was added to a mixture of 3-fluoropicolinic acid (162 mg, 1.15 mmol) in anhydrous CH2Cl2 (3 mL). The mixture was cooled in an ice bath and then treated with oxalyl chloride (0.1 mL, 1.14 mmol) dropwise. The reaction mixture was warmed to r.t. overnight. A mixture of 3-chloro-N1-methyl-4-nitrobenzene-1,2-diamine (Intermediate 2, 208 mg, 1.03 mmol) and triethylamine (0.16 mL, 1.15 mmol) in anhydrous CH2Cl2 (3 mL) was then added, and the mixture was stirred at r.t. for 2 hrs. The solvent was concentrated under vacuum, and the residue was dissolved in DMSO (2 mL) and stirred at 60 C. for 3 hrs. After cooling to r.t., water was added and the solid precipitate was collected via filtration, washed with water, and air dried. The crude product obtained was used directly in the next step without further purification.; This compound was prepared according to a modified procedure described for Intermediate 3, using 3,5-difluoroisonicotinic acid instead of 3-fluoropicolinic acid as starting material. Following the addition of DMSO, concentrated HCl (1 mL) was added and the mixture was stirred at 80 C. for 3 hrs. LCMS calculated for C13H8ClF2N4O2 (M+H)+: m/z=325.0; Found: 324.9.
At the same time, in my other blogs, there are other synthetic methods of this type of compound,903522-29-2, 3,5-Difluoroisonicotinic acid, and friends who are interested can also refer to it.
Reference:
Patent; Incyte Corporation; Hummel, Joshua; Nguyen, Minh; Sokolsky, Alexander; Vechorkin, Oleg; Ye, Qinda; Yao, Wenqing; (72 pag.)US2019/315717; (2019); A1;,
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