Simple exploration of 2,6-Dichloro-3-nitrobenzonitrile

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 5866-98-8 as follows. name: 2,6-Dichloro-3-nitrobenzonitrile

To a 1 L two-neck round bottom flask was added 2,6-dichloro-3-nitrobenzonitrile (11. I g, 51.1 mmol) followed by ethyl acetate (102 mL). The flask was equipped with an internal thermometer and magnetic stir bar and cooled to 5 0C by immersion into an ice bath. Methylamine was added dropwise to the cooled reaction mixture as a 40% aqueous solution (8.9 mL, 115 mmol) with vigorous stirring. The reaction mixture was stirred for an additional 3 hours with cooling, after which more methylamine (1.8 ?iL, 23 r?mol) was added. The reaction vessel was removed from the ice bath and stirred for an additional 1.5 hours. To the reaction mixture was added water (30 mL) followed immediately by hexane (45 mL) and the resulting slurry was stirred for 15 minutes. The solid was recovered by filtration and washed with water followed by methanol to provide 6-chloro-2-methylamino-3-nitro- benzonitrile (10.49 g, 96%) as a bright yellow solid, which was used directly without further purification. 1H NMR (400 MHz, OMSO-de) delta 8.55 – 8.53 (m, IH), 8.28 (d, IH, J= 9.0 Hz), 6.95 (d, IH), J = 9.0 Hz), 3.30 (d, IH, 7= 5.5 Hz).

According to the analysis of related databases, 5866-98-8, the application of this compound in the production field has become more and more popular.