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. 76005-99-7, name is 2-Methoxy-4-methylpyridin-3-amine. A new synthetic method of this compound is introduced below., Recommanded Product: 76005-99-7
(2) 29.4 g of Compound 2 was dissolved in 600 mL of dichloromethane, 25.0 g of potassium acetate was added,Then, the temperature was lowered to 0 C, 43.4 g of acetic anhydride was slowly added dropwise,After about 40 min, 11.25 g of 18-crown-6 ether was added,After the completion of dropping, 54.9 g of isoamyl nitrite was slowly added dropwise at 0 C, and the temperature was returned to room temperature, and the temperature was raised to 65 C and refluxed overnight. After about 12 h, the reaction mixture was adjusted to pH 6 with saturated sodium hydrogencarbonate solution,The organic phase was separated,The aqueous phase was again extracted once with dichloromethane,The combined organic phase was dried and concentrated.Methanol and potassium carbonate were added to the residue, and the mixture was stirred at room temperature for 1 h. After the reaction was complete, the system was filtered off and dried, and the residue was dissolved in ethyl acetate.Saturated sodium chloride solution, and concentrated to dryness to obtain 29 g of the crude product (Compound 3) in a yield of 91.3%. TLC information (petroleum ether: ethyl acetate = 1: 1): starting material Rf = 0.8, product Rf = 0.5.
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Reference:
Patent; Sphinx Scientific Laboratory Corporation; Yao, Qingjia; Xu, Yangjun; Wu, Simin; (6 pag.)CN103992318; (2016); B;,
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