Electric Literature of 54932-72-8, These common heterocyclic compound, 54932-72-8, name is 4-Bromo-1-chloro-2-methylbenzene, 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.
Under argon, a 250 mL three-necked flask was charged with 19.7 g of 2-chloro-5-bromotoluene (I), 11.7 g of o-aminothiophenol (n), 0.5 g of cuprous chloride, 36.5 g of tetramethylethylenediamine and 50 mL of water,Mechanical stirring, oil bath 130 C, the reaction 18 h.The reaction mixture was cooled to room temperature, extracted with 50 1111> 3 ethyl acetate, 12.5 mL * 3 aqueous ammonia and extracted with 25 mL * 3 purified water three times. The combined ethyl acetate phases were washed with 50 mL of purified water and 15 mL of aqueous ammonia, Brine, dried over anhydrous sodium sulfate. The dried ethyl acetate layer was dried, after adding 25 mL of petroleum ether dissolved, rapidly cooled to -5–10 C under stirring, and accompanied by a large amount of solid precipitation, vacuum filtration, the filter cake with petroleum ether leaching wash. The filter cake was collected and dried under reduced pressure at 40 C to give 2- (2-methyl-4-bromo-phenylmercapto) aniline(1Pi) 16.39 g, yield 83.2%, purity 90.1%.
The synthetic route of 54932-72-8 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Jiangsu Ji Bell Pharmaceutical Co., Ltd.; Ding Deping; Li Zhaoguang; Feng Qi; Tang Zhiqun; Liu Jun; Jiang Bin; (10 pag.)CN107513048; (2017); A;,
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