Electric Literature of 873-38-1, These common heterocyclic compound, 873-38-1, name is 2-Bromo-4-chloroaniline, 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.
To a suspension of 2-bromo-4-chloroaniline (5g, 24.22 mmol) in HCl (36.5%wt, 30 mL, 365 mmol) and water (100 mL) at -5C, a solution of sodium nitrite (1.838 g, 26.6 mmol) in water (10 mL) was added dropwise. The mixture was stirred at -5C for 1 h, and the suspension turn into a clear solution. A solution of sodium azide (1.732 g, 26.6 mmol) in water (10 mL) was added dropwise to the reaction. Solids precipitated out from the solution during the addition. It was stirred at -5C for 0.5 h. The mixture was extracted with ethyl acetate (70 mL x 3). The combined organic layers were washed with saturated aqueous sodium bicarbonate (20 mL), water (40 mL) and brine (50 mL) sequentially. The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to give the title compound.
The synthetic route of 873-38-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; MERCK SHARP & DOHME CORP.; XU, Jiayi; ALI, Amjad; ZHOU, Wei; GAO, Ying-Duo; EDMONDSON, Scott, D.; MERTZ, Eric; NEELAMKAVIL, Santhosh, F.; LIU, Weiguo; SUN, Wanying; SHEN, Dong-Ming; HARPER, Bart; ZHU, Cheng; BARA, Thomas; LIM, Yeon-Hee; YANG, Meng; (227 pag.)WO2017/74832; (2017); A1;,
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