468075-00-5, 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. 468075-00-5 name is 2-Bromo-1-chloro-4-(trifluoromethoxy)benzene, 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.
A suspension of ethyl 2-(3-(2-chloro-5-(trifluoromethoxy)phenyl)-8-methyl-3-azaspiro[5.5]undecan-9-yl)acetate (140 mg, 0.553 mmol), cesium carbonate (540 mg, 1.66 mmol), 2-bromo-1-chloro-4-(trifluoromethoxy)benzene (0.175 ml, 1.105 mmol) and (RuPhos)palladium(II) phenethylamine chloride (40.3 mg, 0.055 mmol) in 1,4-dioxane (3 ml) in amicrowave reaction vial was bubbled with nitrogen. The vial was sealed and the mixture was stirred overnight in an oil bath kept at 100C. The mixture was diluted with aq. NH4Cl solution and extracted 3 times with ethyl acetate. The combined organic layer was washed with brine, dried over MgSO4, filtered and evaporated to dryness. The crude product was purified by chromatography eluting with 0-10%-20% ethyl acetate-hex to give ethyl 2-(3 -(2-chloro-5-(trifluoromethoxy)phenyl)-8-methyl-3-azaspiro[5.5]undecan-9-yl)acetate. LCMS m/z 448.13 [M+H]+.
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Bromo-1-chloro-4-(trifluoromethoxy)benzene, and friends who are interested can also refer to it.
Reference:
Patent; MERCK SHARP & DOHME CORP.; CHELLIAH, Mariappan; CHU, Hong Dong; COX, Jason, M.; DEBENHAM, John, S; EAGEN, Keith; LAN, Ping; LONDON, Clare; PLOTKIN, Michael, A.; SHAH, Unmesh; SINZ, Christopher Joseph; SUN, Zhongxiang; VACCARO, Henry, M.; VENKATRAMAN, Skikanth; WO2014/59232; (2014); A2;,
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