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. 108-48-5, name is 2,6-Dimethylpyridine. A new synthetic method of this compound is introduced below., HPLC of Formula: C7H9N
To 20ml reactor followed by addition of a solvent [Bmim] BF4(2 ml), 2,6- lutidine (1 mmol), inter-cyano benzaldehyde (0.5 mol), the catalyst [Hnhm] HSO4(0.5 mmol), sealed reactor, 100 for 48 hours.After the reaction system was cooled with diethyl ether (2 ml) and extracted 6 times, the combined organic phases, the organic phase was dried over anhydrous magnesium sulfate, the organic phase by rotary evaporation to give the crude product.The crude product with petroleum ether: ethyl acetate = 3: 1 (v / v) as eluent and silica gel as the adsorption phase column chromatography, to obtain a solid productC2, Yield 80%. Since the catalyst and a solvent used for the reaction can be recycled after extraction system vacuum dried at 40 degrees Celsius for one hour, then sequentially added 2,6-lutidine (1 mmol), inter-cyano benzaldehyde (0.5 mol ), sealed heating 48 hours, the product was isolatedC2Yield 81%.And so, the catalyst cycle times can still use 8 to 80% yield of the productC2Yield not significantly reduced, indicating that the catalyst for this reaction can be recycled, greatly reducing the cost of the experiment, reducing waste emissions and environmental pollution. NMR data:1the H NMR (400 MHz, CDCl3, TMS) delta 7.60 -7.47 (m, 5H), 7.03 (d,J= 7.6 Hz, 1H), 6.86 (d,J=7.6Hz,1H),5.16(dd,J=3.2,8.8Hz,1H),2.96-3.08(m,2H),2.53(s,3H);13CNMR(400MHz,CDCl3TMS) delta158.8, 157.5, 149.7, 137.5, 132.2, 126.6, 121.7, 120.7, 119.0, 110.9, 72.7, 44.6, 24.3
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Reference:
Patent; Qingdao Agricultural University; WANG, ZU-LI; ZHANG, XUE-YAN; DONG, DAO-QING; (8 pag.)CN104072406; (2016); B;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem