Reference of 56961-77-4, A common heterocyclic compound, 56961-77-4, name is 1-Bromo-2,3-dichlorobenzene, molecular formula is C6H3BrCl2, 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.
Intermediate 1-1 was synthesized according to the following reaction formula. To a 2 L flask was added 1-bromo-2,3-dichlorobenzene (55.0 g, 0.243 mol) and sodium tert-butoxide (72.5 g, 0.755 mol) with 700 mL of toluene and the mixture was refluxed for one hour and stirred. After cooling to room temperature, aniline (45.1 g, 0.485 mol) was added and the temperature was raised. After adding 2,2′-bis (diphenylphosphino) -1,1′-binaphthalene (rac-BINAP) (6.06 g, 9.74 mmole), tris (dibenzylideneacetone) dipalladium (0) (4.46 g, 0.284 mol) dissolved in 30 mL of toluene was slowly added dropwise. After completion of the reaction, the reaction mixture was cooled to room temperature, extracted with ethyl acetate and water, and the obtained organic layer was treated with anhydrous magnesium sulfate, filtered and concentrated to obtain the desired product. Intermediate 1-1 (36.0 g, yield 50%) was obtained by column chromatography using ethyl acetate and hexane.
The synthetic route of 56961-77-4 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; LG Chem, Ltd.; Gu Gi-dong; Lee Gi-gon; Kim Gong-gyeom; Kim Hyeong-seok; Hwang Seong-seok; Lee Sang-u; (28 pag.)KR2019/37174; (2019); A;,
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