Synthetic Route of 452-63-1, 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. 452-63-1 name is 1-Bromo-4-fluoro-2-methylbenzene, 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.
To a solution of bis (dibenzylidene acetone) palladium (0) (0.719 g, 1.25 mmol) and tris (2-methylphenyl) phosphine (0. 761 g, 2. 50 mmol) in toluene (150 mL) were added sodium tert- butoxide (3. 36 g, 35.0 mmol), 2-BROMO-5-FLUOROTOLUENE (3.16 mL, 25.0 mmol) and tert-butyl 1-piperazinecarboxylate (5.03 g, 27.0 mmol) at room temperature, and the mixture was stirred under a nitrogen atmosphere at 100C for 20 hrs. After cooling, the reaction mixture was washed with water and saturated brine, dried (MGS04) and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (developing solvent: hexane/ethyl acetate = 9/1) to give the title compound as a yellow oil (2.50 g, yield 34%). 1H NMR (300 MHz, CDC13) 8 PPM : 1.49 (s, 9 H), 2.30 (s, 3 H), 2.77-2. 80 (m, 4 H), 3.54-3. 57 (m, 4 H), 6.80-6. 96 (m, 3 H). LC/MS (ESI) m/z 295 (M+H+).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-4-fluoro-2-methylbenzene, and friends who are interested can also refer to it.
Reference:
Patent; TAKEDA CHEMICAL INDUSTRIES, LTD.; WO2004/46107; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary