Continuously updated synthesis method about 399-94-0

The synthetic route of 399-94-0 has been constantly updated, and we look forward to future research findings.

Application of 399-94-0, A common heterocyclic compound, 399-94-0, name is 1-Bromo-2,5-difluorobenzene, molecular formula is C6H3BrF2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Description 14:; 2-Bromo-3,6-difluorobenzaldehyde (D14)To solution of diisopropylamine (13.29 mL, 93 mmol) in THF (300 mL) at -78 0C, was added n-butyllithium (34.2 mL of 2.5M in hexanes, 85 mmol), dropwise over 10 mins. The mixture was stirred at -78 0C for 15 mins and then 2-bromo-1 ,4-difluorobenzene (15 g, 78 mmol) in THF (100 mL) was added dropwise over 15 mins maintaining the temperature below -65 C. After stirring for 1 hr at -78 0C, N,N-dimethylformamide (6.62 mL, 85 mmol) was added via syringe. The mixture was stirred at -78 0C for 30 mins and then quenched with sat. NH4CI solution and the mixture was allowed to reach room temperature. The product was extracted into ether and the extracts were dried (Na2SO4) and evaporated. Chromatography (silica, 0-100% dichloromethane in hexane) gave the title compound(D14) as a yellow solid (12.73 g)NMR (deltaH), (CDCI3): 7.16 (1 H, m), 7.35 (1 H, m), 10.32 (1 H, s).

The synthetic route of 399-94-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; WO2008/107455; (2008); A1;,
Bromide – Wikipedia,
bromide – Wiktionary