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. 3430-26-0, name is 2,5-Dibromo-4-methylpyridine. A new synthetic method of this compound is introduced below., Product Details of 3430-26-0
Intermediate 43. Step 1; 5-bromo-4-methylpicolinic acid To a solution of 2,5-dibromo-4-methylpyridine (3 g, 11.96 mmol) in anhydrous toluene (40 ml)) was added BuLi (5.74 ml, 14.35 mmol) at -78 °C dropwise. The reaction mixture was stirred at – 78 °C for 1 h. Then the reaction mixture was poured into a 100 mL beaker with dry carbon dioxide (4 g, 91 mmol). The reaction mixture was stirred at 20 °C for another 10 minutes. Then the mixture was poured into saturated citric acid and a yellow precipitate was formed. The suspension was filtered and the solid was collected, dried in vacuo to give 5-bromo-4- methylpicolinic acid. 1HNMR (400 MHz, DMSO-i): delta = 8.71 (s, 1 H), 7.99 (s, 1 H), 2.40 (s, 3 H). MS: 215.9 (M+l) ppm.
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Reference:
Patent; MERCK SHARP & DOHME CORP.; LIU, Jian; KOZLOWSKI, Joseph, A.; ALHASSAN, Abdul-Basit; BOGA, Sobhana Babu; GAO, Xiaolei; GUIADEEN, Deodialsingh; WANG, Jyhshing; XU, Jiayi; YU, Wensheng; YU, Younong; CAI, Jiaqiang; LIU, Shilan; WANG, Dahai; WU, Hao; YANG, Chundao; (211 pag.)WO2016/109221; (2016); A1;,
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