As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 30766-11-1, name is 5-Bromopicolinic acid, molecular formula is C6H4BrNO2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. Quality Control of 5-Bromopicolinic acid
Step A:5-bromopyridine-2-carboxylic acid (57, 1.0 g, 5.0 mmol)Dissolved in ethylene glycol dimethyl ether (12 mL) and water (4 mL),Add p-fluorophenylboronic acid (17, 1.0 g, 7.5 mmol)And anhydrous potassium carbonate (1.0 g, 7.5 mmol),Then tetrakis(triphenylphosphine)palladium (289 mg, 0.25 mmol) was added.The resulting mixture was stirred at 98 C for 24 hours under a nitrogen atmosphere.TLC analysis indicated that the reaction was over,The reaction solution was cooled to room temperature.Then add water (40 mL),The pH was adjusted to 2-3 with 6M hydrochloric acid.Filtered, the filter cake is dissolved in dichloromethane,The organic layer was washed with 20 mL of saturated sodium bicarbonate solution.Divide the water layer,The aqueous layer was adjusted to pH 2-3 with a 6M hydrochloric acid solution.Filter the solid,The filter cake is washed with water to neutrality.The filter cake was dried to give compound 61 (942 mg).Yield: 87.7%.
With the rapid development of chemical substances, we look forward to future research findings about 30766-11-1.
Reference:
Patent; Zhejiang Haizheng Pharmaceutical Co., Ltd.; Wang Haibo; Zheng Xiaohe; Cai Zhengjiang; Zheng Shan; Ye Zhengchun; Ma Huidan; Lin Haiming; (54 pag.)CN108623532; (2018); A;,
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