These common heterocyclic compound, 1435-51-4, name is 1,3-Dibromo-5-fluorobenzene, 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. 1435-51-4
9H-pyrido[2,3b]indole (5.04 g, 30.00 mmol, 1.0 eq) was sequentially added to a dry reaction tube with a magnetic rotor.CuI (571.4 mg, 3.00 mmol, 0.01 eq),L-Proline (690.0mg,6.00mmol, 0.02eq) andK2CO3 (8.29 g, 60.00 mmol, 2.0 eq).Pumping nitrogen three times,Then added 1,3-dibromo-5-fluorobenzene (9.14 g, 36.0 mmol, 1.2 eq) andSolvent dimethyl sulfoxide (30 mL).The reaction mixture was placed in an oil bath at 120 C for 1.5 days.Cool to room temperature, add 100 mL of ethyl acetate and dilute with Celite.And fully washed with ethyl acetate, added50mL of water, liquid separation, ethyl acetate extraction of the aqueous phase three times, the organic phase was combined, the organic phase was dried over anhydrous sodium sulfate, filtered, the solvent was evaporated under reduced pressure, the crude product was purified by silica gel column chromatography, eluent (petroleum ether) /methylene chloride = 4:1-2:1),Obtained a white solid 2-Br-F 3.22g,The yield was 31%. The product was used directly in the next step of synthesis.
Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 1435-51-4.
Reference:
Patent; Zhejiang University of Technology; Ruisheng Optoelectric Science And Technology (Changzhou) Co., Ltd.; Li Guijie; She Yuanbin; Zhao Xiangdong; Chen Shaohai; (33 pag.)CN108948095; (2018); A;,
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