Electric Literature of 66417-30-9, 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. 66417-30-9 name is 2-Bromo-1-methyl-4-(trifluoromethyl)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.
2-Bromo-4- (trifluoromethyl) toluene (23b, 5g, 21 mmol) was placed in round-bottom flask and dissolved in 150 ml DMF.Then KOAc (6.2g, 63 mmol, 3eq) was added to the reaction mixture in one portion followed by addition of PdCl2 (dppf)(0.46g, 0.63 mmol, 0.03eq) and Bis (pinacolato) diboron 5.9g,23.1 mmol, l.leq). The solution was stirred at 80C for 48h. Then the solvent was removed and the black residue was subjected to plug column chromatography (EtOAc) resulting in dark green oily residue. The compound was further purified by second column chromatography (2% MeOH/DCM) .Pure product (3.5g, 58%) as a slightly green oil was collected.Structure determination:RP-HPLC Conditions: HP 1100 HPLC chromatograph, Waters 3.9 x 150 mm NovaPak HR C18 column with guard column, 0.010 mL injection, 1.5 mL/min, 1.500 mL injection loop, 254 nm detection, A = water (0.1% v/v TFA) and B = MeCN (0.1% v/v
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Bromo-1-methyl-4-(trifluoromethyl)benzene, and friends who are interested can also refer to it.
Reference:
Patent; SENSORS FOR MEDICINE AND SCIENCE, INC.; WO2008/66921; (2008); A2;,
Bromide – Wikipedia,
bromide – Wiktionary