Electric Literature of 133928-73-1, 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. 133928-73-1, name is 2-Chloro-3-methyl-4-pyridinecarboxylic Acid. A new synthetic method of this compound is introduced below.
[01652] Step 4: Synthesis of methyl 2-chl hylpyridine-4-carboxylate[01653] To a stirred solution of 2-chloro-3-methylpyridine-4-carboxylic acid (780 mg, 4.5 mmol) in anhydrous DMF (5.0 ml), was added potassium carbonate (1 .25 g, 9.1 mmol), followed by methyl iodide (0.42 ml, 6.8 mmol) dropwise. A further 4 ml of DMF was added and the reaction mixture was stirred at room temperature under nitrogen for 18.5 hours. The solvent was removed in-vacuo and the residue was then partitioned between CI b b (20 ml) and water (20 ml). The layers were separated and the aqueous layer was extracted with CH2C12 (3 x 15 ml). The combined organic layers were washed with water (2 x 30 ml), brine (40 ml), dried (MgS0 ), filtered and concentrated in-vacuo. The residue was purified by column chromatography (l Og SNAP cartridge, Isolera, 0-6% ethyl acetate:heptanes) to give the title compound (591 mg, 59%) as a colourless oil. LC-MS 84%, m/z = 185.9, 1 87.9; NMR (500 MHz, Chloroform-d) delta ppm 8.33 (d, J=5.04 Hz, 1 H) 7.54 (d, J=5.04 Hz, 1 H) 3.95 (s, 3 H) 2.60 (s, 3 H).
At the same time, in my other blogs, there are other synthetic methods of this type of compound,133928-73-1, 2-Chloro-3-methyl-4-pyridinecarboxylic Acid, and friends who are interested can also refer to it.
Reference:
Patent; EPIZYME, INC.; EISAI CO., LTD.; KUNTZ, Kevin, Wayne; CHESWORTH, Richard; DUNCAN, Kenneth, William; KEILHACK, Heike; WARHOLIC, Natalie; KLAUS, Christine; ZHENG, Wanjun; WO2012/142513; (2012); A1;,
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