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. 709652-82-4, name is 2-Amino-5-bromonicotinonitrile. A new synthetic method of this compound is introduced below., Recommanded Product: 2-Amino-5-bromonicotinonitrile
Step 2: Preparation of 5-bromo-2-(2,5-dimethyl-1H-pyrrol-1-yl) nicotinonitrile (44) To a suspension solution of the intermediate 42 (90.0 g, 0.45 mol, 1.0 eq) in toluene (1.5 L) was added the compound 43 (78.2 g, 0.68 mol, 1.5 eq) and 4-methylbenzenesulfonic acid (2.5 g, 0.01 mol, 0.03 eq). The mixture was heated to 110 C. and stirred for 17 hours to remove water by Dean Stark trap. The mixture was cooled to room temperature, removed of toluene (about 1 L), and then added with EtOAc (2 L) and water (1 L). The mixture was filtered; the aqueous layer was extracted with EtOAc (2 L); the organic phase was washed with brine (3 L) and concentrated to give the crude product, which was purified by flash chromatography (EtOAc:Hexane=1:1) to give the intermediate 44 (110.0 g, 0.39 mol, 87.1%). 1H NMR (400 MHz, DMSO-d6) delta 9.07-9.06 (d, J=2.4 Hz, 1H), 8.96-8.95 (d, J=2.4 Hz, 1H), 5.88 (s, 2H), 2.01 (s, 6H).
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Reference:
Patent; GREEN CROSS CORPORATION; CHOI, Soongyu; PARK, Eun-Jung; SEO, Hee Jeong; KONG, Younggyu; SON, Ickhwan; MA, Sang-ho; CHA, Man-Young; KIM, Mi-Soon; PARK, Kisoo; (143 pag.)US2016/311772; (2016); A1;,
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