With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.40296-46-6, name is Ethyl 4,6-dichloronicotinate, molecular formula is C8H7Cl2NO2, molecular weight is 220.0527, as common compound, the synthetic route is as follows.Product Details of 40296-46-6
Example IX Preparation of [(4,6-dichloropyridin-3-yl)methyl](methyl)-oxido lambda4-sulfanylidenecyanamide (9) To a stirred solution of ethyl 4,6-dichloronicotinate (8.8 g, 40 mmol) in anhydrous THF (75 mL) cooled in an ice-water bath was added in a dropwise fashion 1 M LiAlH4 solution in THF (25 mL, 25 mmol). During the addition, the temperature was not allowed to rise above 25 C. After the addition was over, the reaction was warmed to 40 C. for 15 min, cooled, then quenched by the successive dropwise addition of water (0.95 mL), 15% aqueous NaOH (0.95 mL) and water (1.85 mL). The mixture was filtered through celite and the filtrated was dried (MgSO4), passed through a short pad of silica gel and concentrated to give a red oil. Ether (100 mL) was added whereupon a gummy precipitate immediately appeared, which was removed by filtration. The ether solution was allowed to stand at room temperature overnight, during which time more precipitate was formed which was removed again by filtration. The ether solution was concentrated and dried to give 3.25 g of the product 2,4-dichloro-5-hydroxy-methylpyridine in 46% yield as a nearly colorless oily solid. 1H NMR (300 MHz, CDCl3) delta 8.5 (s, 1H), 7.4 (s, 1H), 4.8 (s, 2H), 2.7 (bs, 1H); GC-MS: mass calcd for C6H5Cl2NO [M]+, 177. Found
At the same time, in my other blogs, there are other synthetic methods of this type of compound,40296-46-6, Ethyl 4,6-dichloronicotinate, and friends who are interested can also refer to it.
Reference:
Patent; Zhu, Yuanming; Loso, Michael R.; Nugent, Benjamin M.; Huang, Jim X.; Rogers, Richard B.; US2008/108667; (2008); A1;,
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