Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 64248-62-0, name is 3,4-Difluorobenzonitrile, A new synthetic method of this compound is introduced below., SDS of cas: 64248-62-0
A well dried 5 L, four necked round bottom flask fitted with over-head stirrer was charged a solution of diisopropyl amine (174.6 mL, 2.3 eq, 826.7 mmol) in THF (400 mL) and cooled to -78C. It was added n-butyllithium (496 mL, 2.3 eq, 1240.1 mmol, 2.5 M solution in hexane) at -78C under nitrogen atmosphere and stirred for 1 h. To the resulting LDA solution was added a mixture of N- nitrosodimethylamine 2 (87.7 g, 2.2 eq, 1 186.1 mmol) and 3,4- difluorobenzonithle (75 g, 1 eq, 539.1 mmol) in THF (1000 mL). The reaction mixture was stirred at -78C for 1 h and then slowly warmed to RT and stirred for additional 4h at RT. The reaction mixture was quenched by the addition of saturated aq. ammonium chloride solution (300 mL), extracted with ethyl acetate (3*300 mL). The combined organic extracts were washed with brine (2*200 mL), dried over anhydrous sodium sulphate and evaporated to afford crude (1 18 g) as a brownish gum. The crude material was purified by column chromatography by using silica gel (60-120 mesh) using 30% ethyl acetate in hexane as eluent, to afford 4-(3,4-difluorophenyl)-1 -methyl-1 H-1 ,2,3-triazole 3 (30 g, 28% yield) as pale yellow solid. 1H NMR (400 MHz, CDCl3): delta 7.73 (s, 1 H), 7.71 -7.64 (m, 1 H), 7.57-7.51 (m, 1 H), 7.28-7.19 (m, 1 H), 4.18 (s, 3H).
The synthetic route of 64248-62-0 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ANIONA APS; LARSEN, Janus Schreiber; GUSTAFSSON, Magnus; JESSEN, Carsten; WO2014/1278; (2014); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts