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. 126717-59-7, name is 3-Bromo-6-methoxy-2-picoline. A new synthetic method of this compound is introduced below., HPLC of Formula: C7H8BrNO
The compound 3-bromo-6-methoxy-2-methylpyridine (15 g, 0.076 mol), N-bromosuccinimide (40 g, 0.22 mol),Tetrahydrofuran (100 mL), acetic acid (7.5 mL),Azobisisobutyronitrile (0.45 g, 2.7 mmol) was added to a 500 ml single-mouth flask equipped with a reflux apparatus, and the reaction system was heated to reflux for 12 hours.Cool to room temperature and add ethyl acetate (150 mL).Adjust the pH to about 8 with a saturated aqueous solution of sodium bicarbonate (40 mL).The organic phase was washed with saturated brine (30 mL) and dried over anhydrous sodium sulfate.Dry to give a clear oily mixture of compound 3-bromo-2-(dibromomethyl)-6-methoxypyridine and 3-bromo-2-(bromomethyl)-6-methoxypyridine (26 g ),Used directly in the next step.3-Bromo-2-(dibromomethyl)-6-methoxypyridine in sequence at room temperaturea mixture with 3-bromo-2-(bromomethyl)-6-methoxypyridine (26 g),Anhydrous tetrahydrofuran (100 mL), N,N-diisopropylethylamine(25.8 mL, 0.19 moL), added to a 500 ml three-neck bottle,Nitrogen protection, cooling to 0 C, diethyl phosphite(18.6 mL, 0.14 mol) was added dropwise to the reaction system.After completion, the reaction solution was stirred at normal temperature for 12 hours.Ethyl acetate (200 mL) was added to the reaction system.Wash twice with saturated brine (20 mL) and dry over anhydrous sodium sulfate.Spin dry, pass through the column (petroleum ether (v) / ethyl acetate (v) = 50:1)3-bromo-2-(bromomethyl)-6-methoxypyridine (15.5 g, two-step yield: 77%)Transparent oil.
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Reference:
Patent; Wanbangde Pharmaceutical Group Co., Ltd.; Zhang Kai; (10 pag.)CN104151240; (2017); B;,
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