In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 936841-69-9, name is 4-(Trifluoromethyl)picolinonitrile, the common compound, a new synthetic route is introduced below. Quality Control of 4-(Trifluoromethyl)picolinonitrile
To a solution of 4-(trifluoromethyl)pyridine-2-carbonitrile (0.516 g, 3.00 mmol) in methanol (4.5 ml) was added sodium methoxide (30 wt% in MeOH) (0.027 g, 0.150 mmol, 0.028 ml). The mixture was stirred at room temperature for 3 h. The solution was transferred into a reaction vial, methylamine (33 wt% inEtOH) (1.512 g, 16.07 mmol, 2.0 ml) was added, the vial was closed and the mixture was heated at60C overnight. Hydrochloric acid (4M in dioxane) (3.00 mmol, 0.750 ml) was added and heating was continued at 90C for 2 h. The reaction mixture was concentrated. In a reaction vial, the residue was redissolved in methylamine (33 wt% in EtOH) (7.56 g, 80 mmol, 10.00 ml), hydrochloric acid (4M in dioxane) (3.00 mmol, 0.750 ml) was added, the vial was capped and the mixture was heated at 90Covernight. The reaction mixture was concentrated and the residue partitioned between diethyl ether and sat. Na2CO3 (aq). After washing and separation of the phases, the aqueous layer was extracted with ether two more times. The combined organic layers were dried over sodium sulfate and concentrated. The residue was purified over silica by flash column chromatography (0-100% B in A; A: CH2CI2 B: CH2CI2/MeOH/Et3N, 9/1/0.1). The fractions containing product were combined andconcentrated. The residue was dissolved in methanol and hydrochloric acid in dioxane (4M, 2 ml) was added. The mixture was concentrated, coevaporated with methanol and twice with diethyl ether to afford the title compound (484 mg) as a solid. LCMS (method 1): 218 (M+H), retention time 1.47 mm. 1H-NMR (DMSO-d6, ppm) 2.86 (3H), 3.06 (3H), 8.15 (1H), 8.29 (1H), 9.09 (1H), 9.87 (1H), 10.23 (1H).
The synthetic route of 936841-69-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; SYNGENTA PARTICIPATIONS AG; MUEHLEBACH, Michel; TITULAER, Ruud; EMERY, Daniel; EDMUNDS, Andrew; STOLLER, Andre; JUNG, Pierre Joseph Marcel; BUCHHOLZ, Anke; RENOLD, Peter; (98 pag.)WO2015/144826; (2015); A1;,
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