Reference of 202865-58-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 202865-58-5 name is 1-Bromo-4,5-difluoro-2-methoxybenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
Add trifluoromethanesulfonic acid 6-methoxy-1- [4- (2-piperidin-1-yl-ethoxy)- benzoyl] -naphthalen-2-yl ester (2.3 gm, 4.2 mmoles), bis (pinacolato) diboron (1.3 gm, 5.1 mmoles), palladium II acetate (97 mg, 0. 4 mmoles), triphenylphosphine (222 mg, 0.84 mmoles) and cesium fluoride (2.1 gm, 14.1 mmoles) in a 250 ml round bottom flask under nitrogen and add 100 ml of anhydrous acetonitrile. Stir and heat to reflux for 2 hours. Allow the mixture to cool and to this mixture add 2-bromo-4,5-difluoroanisole (2.8 gm, 12.5 mmoles), palladium II acetate (96 mg, 0.43 mmoles) triphenylphosphine (222 mg, 0.84 moles) and cesium fluoride (1.8 gm, 12.2 mmoles). Reflux the mixture for 18 hours and filter through Celite. Evaporate the solvent and pass through an SCX column eluting the product with 2N ammonia/methanol. The product is purified on a silica column eluting with a gradient of 25% THF/hexane to 5% 2N ammonia/methanol in 25 % THF/Hexane. LC/MS gives a peak with the proper mass.
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-4,5-difluoro-2-methoxybenzene, and friends who are interested can also refer to it.
Reference:
Patent; ELI LILLY AND COMPANY; WO2005/73204; (2005); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem