Synthetic Route of 1435-51-4, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 1435-51-4, name is 1,3-Dibromo-5-fluorobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.
1,3-Dibromo-5-fluoro-benzene (20 g, 78.77 mmol, 1 eq) was dissolved in i-Pr2O (200 mL) in a dried flask under nitrogen. The reaction mixture was cooled to -78 C and stirred under nitrogen atmosphere. n-BuLi (2.5 M, 31.5 mL, 1 eq) was added drop wise to the above solution and the reaction mixture was stirred at -78 C for 30 min. After complete addition of n-BuLi, N-methoxy-N-methyl-acetamide (9.75 g, 94.5 mmol, 10.05 mL, 1.2 eq) dropped to the above reaction mixture, while keeping the reaction mixture below -78 C. After addition, the reaction mixture was warmed slowly to 30 C for 30 min. The reaction mixture was poured into water (150 mL) and the reaction mixture was stirred for 15 min. The organic phase was separated and the aqueous phase was extracted with ethyl acetate (150 mL), combined organic phase, dried over anhydrous Na2SO4, filtered and evaporated in vacuum to give residue (16 g crude). The residue was purified by flash silica gel chromatography (ISCO; 120 g CombiFlash Silica Flash Column, Eluent of 0~10% Ethyl acetate/Petroleum ether gradient 85 mL/min). Compound was obtained as off-white solid (11.3 g, yield 66%).1H NMR (400 MHz, CDCl3) delta ppm 7.91 – 7.84 (m, 1H), 7.63 – 7.54 (m, 1H), 7.45 (td, J=2.0, 7.8 Hz, 1H), 2.63 – 2.55 (m, 3H).
The synthetic route of 1,3-Dibromo-5-fluorobenzene has been constantly updated, and we look forward to future research findings.
Reference:
Patent; SAINT LOUIS UNIVERSITY; INDALO THERAPUETICS, INC.; RUMINSKI, Peter, G.; GRIGGS, David, W.; SEIWERT, Scott; (155 pag.)WO2018/132268; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary