Some common heterocyclic compound, 156682-52-9, name is 1,4-Dibromo-2,3-difluorobenzene, molecular formula is C6H2Br2F2, 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. HPLC of Formula: C6H2Br2F2
Preparation of iso-PrMgCl-LiCl-A sample of LiCl (4.56 g, 107.6 mmol) was dried under high vacuum with a heat gun for 10 min. To the dry solid under a N2 atmosphere at 23 C. was added iso-PrMgCl (53.8 mL, 107.6 mmol, 2M solution in THF) and the resulting mixture was stirred at 23 C. for 3 days.To a solution of D-1c (1.29 mL, 10 mmol) in THF (5 mL) at 40 C. was added the iso-PrMgCl-LiCl solution (5.5 mL, 11 mmol, 2.0M in THF) at a rate that maintained the reaction temperature below -30 C. Stirring was continued at -35 to -30 C. for 1 h then warmed to -7 C. for an additional 1 h. The reaction mixture was cooled to -30 C. and DMF (1.00 mL, 13 mmol) was added in one portion (temperature rose to -23 C.) and stirring continued for 3.5 h at -25 to +15 C. The reaction mixture was poured into 1M H2SO4 and ice and the resulting mixture was saturated with solid NaCl and twice extracted with MTBE. The combined extracts were dried (MgSO4), filtered and concentrated in vacuo to afford 2.17 g (98%) of D-1d as a white solid.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 156682-52-9, its application will become more common.
Reference:
Patent; Roche Palo Alto LLC; US2008/249151; (2008); A1;,
Bromide – Wikipedia,
bromide – Wiktionary