Reference of 6515-09-9, 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. 6515-09-9, name is 2,3,6-Trichloropyridine. A new synthetic method of this compound is introduced below.
Step A. (3,6-dichloro-pyridin-2-yl)-acetic acid ethyl ester Malonic acid t-butyl ester ethyl ester (7.1 mL, 36 mmol) was added via syringe over one minute with swirling to a frozen mixture of NaH (968 mg, 38.3 mmol) in DMSO (10 mL) at 0 C. The ice bath was removed and the mixture was stirred at rt for 15 min, and then at 115 C. for less than a minute until H2 evolution had subsided, and was then allowed to cool to rt. A solution of 2,3,6-trichloropyridine (3.26 g, 17.9 mmol) (J. Chem. Soc. C: Organic 1375, 1970) in DMSO (12 mL) was added, and the reaction stirred at 115 C. for 4 h. The reaction was then cooled to rt, shaken with 0.5 M NaH2PO4 (100 mL), and extracted with ether (1*50 mL; 2*25 mL). The organic layers were combined, washed with brine (1*20 mL), dried (Na2SO4), and concentrated under high vac at 95 C. to give a mixture of dichloro-pyridin-2-yl-malonic acid tert-butyl ester ethyl ester regioisomers as a clear amber oil (6.40 g) that was immediately used in the next step without further purification or characterization.
At the same time, in my other blogs, there are other synthetic methods of this type of compound,6515-09-9, 2,3,6-Trichloropyridine, and friends who are interested can also refer to it.
Reference:
Patent; Player, Mark R.; Lu, Tianbao; Hu, Huaping; Zhu, Xizhen; Teleha, Christopher; Kreutter, Kevin; US2007/225282; (2007); A1;,
Pyridine – Wikipedia,
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