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 698-00-0 as follows. name: 2-Bromo-N,N-dimethylaniline
General procedure: In a fume hood, an oven-dried Schlenk flask equipped with magnetic stirring bar was filled with N2 and evacuated (three cycles). Under N2 atmosphere, Pd(OAc)2 (1.1 mg, 0.005 mmol, 1 mol% Pd), SPhos (4.1mg, 0.01 mmol, 2 mol%), K3PO4 (160 mg, 1.5 mmol, 1.5 equiv), 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-2,6-bis(trifluoromethyl)pyridine (1, 171 mg, 0.5 mmol, 1 equiv), aryl bromide (0.75 mmol,1.5 equiv), and DME (2 mL) were added in order. The Schlenk flask was closed and the mixture was heated at 80 C in an oil bath for 24-48 h. The progress of reaction was monitored by GC-MS and TLC. Upon completion of reaction, the Schlenk flask was cooled to r.t. and exposed to air. The mixture was extracted into EtOAc, washed with water and brine, and dried (anhyd Na2SO4). The crude product was purified by column chromatography (silica gel). For chloro-substituted bromoarenes (2g, 2h, and 2m), Pd(PPh3)4 (23mg, 0.02 mmol, 4 mol% Pd) was used (for 1-mmol scale reaction) in place of Pd(OAc)2 and SPhos. Unless otherwise noted, reactions were performed on a 0.5-mmol 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-2,6-bis(trifluoromethyl)pyridine (1) scale.
According to the analysis of related databases, 698-00-0, the application of this compound in the production field has become more and more popular.
Reference:
Article; Batool, Farhat; Emwas, Abdul-Hamid; Gao, Xin; Munawar, Munawar A.; Chotana, Ghayoor A.; Synthesis; vol. 49; 6; (2017); p. 1327 – 1334;,
Bromide – Wikipedia,
bromide – Wiktionary