Synthetic Route of 5469-19-2, 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. 5469-19-2 name is 1-Bromo-2,4,5-trimethylbenzene, 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.
i 2,4,5-Trimethylbenzoic acid n-Butyllithium (100 ml of a 2.5M solution in hexanes) was added to a solution of 5-bromo-1,2,4-trimethylbenzene (50 g) in tetrahydrofuran (600 ml) at -70 C. After 1.5 hours the solution was warmed to -40 C. then cooled to -70 C. Carbon dioxide gas was bubbled through the solution for 10 minutes and the mixture was allowed to warm to room temperature. The solvent was evaporated and the residue partitioned between water and isohexane. The aqeous layer was acidified to pH 1 and extracted with dichloromethane. The organic solution was dried (MgSO4) and evaporated under reduced pressure. Yield 36.7 g. 1H NMR: delta (CDCl3) 7.85(s, 1H), 7.04(s, 1H), 2.59(s, 3H), 2.28(s, 3H), 2.27(s, 3H)
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-2,4,5-trimethylbenzene, and friends who are interested can also refer to it.
Reference:
Patent; AstraZeneca U.K. Limited; US6162808; (2000); A;,
Bromide – Wikipedia,
bromide – Wiktionary