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. 1221171-70-5, name is 2-Chloro-6-(trifluoromethoxy)pyridine. A new synthetic method of this compound is introduced below., SDS of cas: 1221171-70-5
c) 6-chloro-2-(trifluoromethoxy)-3-(trimethylsilyl)pyridine (1-6); A LDA solution was prepared from n-BuLi 2.5M in hexane (22 mL; 56.80 mmol; 1.1 eq) and diisopropylamine (8 mL; 56.80 mmol; 1.1 eq) in THF (40 mL) at 0C. To the LDA solution at -78 C, a solution of 2-chloro-6-(trifluoromethoxy)pyridine (10.2 g; 51.64 mmol; 1 eq) in THF (40 mL) was added dropwise over 30 minutes. The solution was stirred at -78 C for 2 hours, after what TMSCI (7.20 mL; 56.80 mmol; 1.1 eq) was added dropwise. The reaction mixture was allowed to warm up to room temperature and stirred 1 hour. Water (120 mL) was then added. The aqueous layer was extracted with diethylether (3 x 120 mL), and the combined organic layers were dried over sodium sulphate, filtered and concentrated under reduced pressure. The crude was purified on silica gel using petroleum ether (100 %) as an eluent to afford 6-chloro-2- (trifluoromethoxy)-3-(trimethylsilyl)pyridine in 94 % yield as a colorless oil.1H- MR (CDC13): delta (ppm) 0.33 (s, 9H); 7.21 (d, 1H); 7.77 (d, 1H).
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Reference:
Patent; VIVALIS; CIAPETTI, Paola; TROUCHE, Nathalie; VENKATA PITHANI, Subhash; GUEDAT, Philippe; BERECIBAR, Amaya; WO2012/93174; (2012); A1;,
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