Application of 328-70-1,Some common heterocyclic compound, 328-70-1, name is 1-Bromo-3,5-bis(trifluoromethyl)benzene, molecular formula is C8H3BrF6, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
General procedure: Inside an argon atmosphere glove box, halide (0.5mmol), boronic acid (0.75mmol), K3PO4 (1.5mmol), PPPd (4mg, 1.4wt% Pd, 0.0005mmol), solvent (2ml, H2O/EtOH v/v=2:3) were mixed in a 5ml vessel and sealed. Then it was moved out of the glove box and heated in an oil bath to 80C for 2-6h. After cooled down to r.t. for about half an hour, the mixture was filtered. Take a small amount of the liquid for GC analysis. The solid part was washed three times with ethanol. The combined liquid was dried and purified by column to give pure coupling product. For recycle experiments, the solid part after washing was degassed and used into the next cycle. Combing the recycled catalyst from X reaction times was marked as Re-PPPd-X.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-3,5-bis(trifluoromethyl)benzene, its application will become more common.
Reference:
Article; Wang, Xinbo; Min, Shixiong; Das, Swapan K.; Fan, Wei; Huang, Kuo-Wei; Lai, Zhiping; Journal of Catalysis; vol. 355; (2017); p. 101 – 109;,
Bromide – Wikipedia,
bromide – Wiktionary