Extracurricular laboratory: Synthetic route of 3,5-Difluoropicolinonitrile

The chemical industry reduces the impact on the environment during synthesis 298709-29-2, I believe this compound will play a more active role in future production and life.

Related Products of 298709-29-2, 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.298709-29-2, name is 3,5-Difluoropicolinonitrile, molecular formula is C6H2F2N2, molecular weight is 140.0903, as common compound, the synthetic route is as follows.

A solution of methylmagnesium bromide (36.8 ml, 117.78 mmol) in THF (50ml) was stirred under N2 and cooled to -78C. 3,5-Difluoropicolinonitrile (15.0 g, 107.07 mmol) in THF (50 ml) was added drop wise with an addition funnel at such a rate that the internal temperature was kept below -4C. After the addition was complete, the reaction mixture was poured into a IM HCl (100 ml, chilled in an ice bath). The reaction mixture was stirred at 00C for 30 minutes and room temperature for 30 minutes. To this solution 150 ml of EtOAc was added to extract product. The aqueous phase was neutralized to pH 9 with NaHCO3 and extracted with EtOAc (2 X 20 ml). The organic layers were combined and the volatiles were removed under reduced pressure. Purification by ISCO (0-10% EtOAc- hexanes) gave the title product as light yellow oil. LCMS: 158 [M+H]

The chemical industry reduces the impact on the environment during synthesis 298709-29-2, I believe this compound will play a more active role in future production and life.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2009/150462; (2009); A1;,
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