Related Products of 332-25-2, 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. 332-25-2 name is 4-(Trifluoromethoxy)benzonitrile, 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.
Step 2:; To a stirred solution of N,N-diethyl-4-methoxy-2-methyl-benzamide (10.0 g, 45.2 mmol) in THF (150 mL) at -78° C. under nitrogen atmosphere was added t-BuLi (29.2 mL of 1.7M in pentane, 49.7 mmol) dropwise. The resulting red solution was kept at this temperature for additional 10 min before dropwise addition of 4-(trifluoromethoxy)-benzonitrile (9.49 g, 49.7 mmol). The brown solution was stirred at -78° C. for 2 h; tests by LCMS showed incomplete reaction. Thus to the mixture was added an additional amount of 4-(trifluoromethoxy)-benzonitrile (3.38 g, 18.1 mmol) and the resulting mixture was stirred for an additional 1 h. The mixture was then allowed to warm to rt and was quenched by pouring into aqueous 1.0M HCl (50 mL). EtOAc (100 mL) was added and the mixture was shaken and phases were separated. A precipitate occurred within the EtOAc phase which was isolated by filtration and allowed to dry (3.0 g). This 3.0 g of isolated solid was determined to be impure product and was set aside for later purification. The EtOAc filtrate was set aside. The aqueous acid washes were combined and extracted with DCM (3.x.100 mL). The DCM extracts were combined, washed with brine, dried over MgSO4, filtered and concentrated in vacuo. This residue was combined with the original EtOAc filtrate and the combined organics were concentrated to a slurry. A solid was isolated by filtration to give the desired product (8.84 g, 58.0percent yield). LC-MS, MS m/z 336 (M++H).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-(Trifluoromethoxy)benzonitrile, and friends who are interested can also refer to it.
Reference:
Patent; Bristol-Myers Squibb Company; US2008/119461; (2008); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts