Adding a certain compound to certain chemical reactions, such as: 951624-83-2, 5-(Trifluoromethyl)nicotinonitrile, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, HPLC of Formula: C7H3F3N2, blongs to pyridine-derivatives compound. HPLC of Formula: C7H3F3N2
(Reference Example 117) 6-Chloro-5-(trifluoromethyl)pyridine-3-carbonitrile[0812] Urea hydrogen peroxide (0.815 g, 8.66 mmol) and trifluoroacetic anhydride (1.15 mL, 8.24 mmol) were added to a solution of 5-(trifluoromethyl)pyridine-3-carbonitrile (compound described in the pamphlet of WO2009/42694, 0.71 g, 4.12 mmol) in dichloromethane (10 mL), and the mixture was stirred overnight. A 10% sodium thiosulfate aqueous solution was added to the reaction solution, followed by extraction with dichloromethane twice. The organic layer was washed with brine and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography [elute: hexane/ethyl acetate = 88/12 – 0/100 (gradient)] to obtain a product. [0814] A solution of the obtained product in phosphoryl chloride (10 mL) was stirred at 70C for 2 hours and further for 2 hours under reflux. The reaction solution was poured to ice, followed by extraction with dichloromethane twice. Combined organic layers were washed with brine and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography [elute: hexane/ethyl acetate = 99/1 – 90/10 (gradient)] to obtain the title compound (62 mg, yield: 7%).[0815] 1H-NMR (CDCl3) delta: 8.86 (1H, d, J = 2 Hz), 8.28 (1H, d, J = 2 Hz).
At the same time, in my other blogs, there are other synthetic methods of this type of compound,951624-83-2, 5-(Trifluoromethyl)nicotinonitrile, and friends who are interested can also refer to it.
Reference:
Patent; Daiichi Sankyo Company, Limited; KOBAYASHI, Hideki; OHKAWA, Nobuyuki; TAKANO, Daisuke; KUBOTA, Hideki; ONODA, Toshio; KANEKO, Toshio; ARAI, Masami; TERASAKA, Naoki; EP2862861; (2015); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem