Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 126325-50-6, name is 3-Amino-2-bromo-4-picoline. A new synthetic method of this compound is introduced below., COA of Formula: C6H7BrN2
To a cooled (13 C) mixture of 3-amino-2-bromo-4-picoline (4.5 g, 24.06 mmol, Combi-Blocks) and potassium acetate (3.09 g, 31.5 mmol) in AcOH (100 mL) was added a solution of sodium nitrite (2.01 g, 29.1 mmol) in water (10 mL) dropwise. Upon complete addition the reaction mixture was allowed to slowly warm to rt for 66 h. A solution of NaN02 (706 mg) in water (3 mL) was added to the reaction mixture and the reaction mixture was stirred for 5 h. The solvent was removed under reduced pressure and the residue was basified with saturated NaHC03. The aqueous layer was extracted with EtOAc (3x) and the combined organic layers were washed with water then brine, and dried over MgS04. The filtrate was purified by silica gel flash chromatography, eluting with EtOAc:hexanes (0: 1? 1 :1) to give a white crystalline solid (1.38 g, 7.0 mmol, 29%).MS m/z=198 [M+H]+. Calculated for C6H4BrN3: 198
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Reference:
Patent; AMGEN INC.; MINATTI, Ana Elena; LOW, Jonathan, D.; ALLEN, Jennifer, R.; AMEGADZIE, Albert; BROWN, James; FROHN, Michael, J.; GUZMAN-PEREZ, Angel; HARRINGTON, Paul, E.; LOPEZ, Patricia; MA, Vu Van; NISHIMURA, Nobuko; QIAN, Wenyuan; RUMFELT, Shannon; RZASA, Robert, M.; SHAM, Kelvin; SMITH, Adrian, L.; WHITE, Ryan; XUE, Qiufen; WO2014/138484; (2014); A1;,
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