Synthetic Route of 127446-34-8, 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. 127446-34-8, name is N-(6-Chloro-3-formylpyridin-2-yl)pivalamide. A new synthetic method of this compound is introduced below.
To a solution of Lambda/-(6-chloro-3-formylpyridin-2-yl)pivalamide (prepared as described in J. Org. Chem. (1990), 55, 4744; 3.0 g, 12.64 mmol) in MeCN (250 niL) was added triethyl 2-fluoro-phosphonoacetate (4 g, 16.51 mmol), lithium chloride (0.935 g) and DBU (2.8 mL, 18.7 mmol). The mixture was stirred at rt for 4 h. The solvent was evaporated and the residue was partitioned between N HCl (100 mL) and ether (150 mL). The aq. layer was extracted with ether (10O mL) and the combined ethereal layers were dried over Na2SO4, filtered and concentrated to dryness. The residue was taken up in dioxane (15 mL) and 6JV EtaC1 (50 mL) was added. The mixture was heated to reflux for 90 min. The mixture was cooled to 00C and the volatiles were removed in vacuo. The solids were filtered off and washed with water. The solid was dried in vacuo to afford the title compound as a yellow solid (1.38 g, 56% yield). The title compound was only 70% pure. MS (ESI, m/z): 199.1 [M+Eta+] for C8H4N2OClF.
At the same time, in my other blogs, there are other synthetic methods of this type of compound,127446-34-8, N-(6-Chloro-3-formylpyridin-2-yl)pivalamide, and friends who are interested can also refer to it.
Reference:
Patent; ACTELION PHARMACEUTICALS LTD; HUBSCHWERLEN, Christian; RUEEDI, Georg; SURIVET, Jean-Philippe; ZUMBRUNN ACKLIN, Cornelia; WO2010/116337; (2010); A1;,
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