Reference of 142808-15-9,Some common heterocyclic compound, 142808-15-9, name is 4-Bromo-2-fluorobenzotrifluoride, molecular formula is C7H3BrF4, 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.
Preparation of 3-fluoro-4-trifluoromethylmagnesium bromide:Under nitrogen protection, add 24g of magnesium chips and 100mL of THF to a 2L four-necked flask, first add 3-fluoro-4-trifluoromethylbromobenzene 13g.The reaction was initiated at about 30 C. After the initiation, a solution of 230 g of 3-fluoro-4-trifluoromethylbromobenzene and 700 mL of THF was added dropwise at 40 C, and the mixture was dropped about 2 h.After the completion of the dropwise addition, the mixture was stirred at 50 C for 2 h, and the reaction was monitored by GC, and the raw material was converted to over 99.0%.Preparation of 2-amino-5-methyl-3′-fluoro-4′-trifluoromethyl-1,1′-biphenyl:Prepared 206 g of N-benzylidene-2-chloro-4-methylaniline and 10 g of anhydrous NiCl2 under nitrogen protection.Sphos 20g and THF 500mL were added to a 2L four-necked flask, and the prepared Grignard reagent was dropped into the reaction system at 50 C, and there was a significant exotherm. After the completion of the dropwise addition, the mixture was stirred for 3 hours.200 mL of 30% sulfuric acid was added and stirred at 50 C for 2 h.After removing THF under reduced pressure, the system was cooled to 0 C.Suction filtration to give a brown solid, the crude product is recrystallized from toluene and hepbrowne to give a slightly brown solid powder 215g, 99.0%, yield: 80.0%.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Bromo-2-fluorobenzotrifluoride, its application will become more common.
Reference:
Patent; Shanghai Kangpeng Technology Co., Ltd.; Zeng Yuan; Zhou Yan; Li Bolan; Chen Xiaobin; Wang Daoxiang; Yang Jianhua; (19 pag.)CN108276294; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary