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. 109-85-3, name is 2-Methoxyethylamine, A new synthetic method of this compound is introduced below., category: ethers-buliding-blocks
EXAMPLE 532-[2-(1 ,3-benzothiazol-5-yl)-1 H-imidazol-4-yl]-1 -[2-(methyloxy)ethyl]-1 H-benzimidazole-6- carbonitrile hydrochlorideStep 1 . 5-bromo-N-[2-(methyloxy)ethyl]-2-nitroaniline: 4-bromo-2-fluoro-1 -nitrobenzene (0.3 g, 1.336 mmol), 2-(methyloxy)ethylamine (0.1 17 ml_, 1.336 mmol), and DIEA (0.238 ml_, 1 .336 mmol) in Ethanol (5 mL) were irradiated by microwave at 100C for 30 min. The reaction mixture was partitioned between dichloromethane and brine. The aqueous layer was extracted with DCM twice. The combined DCM layers were dried over sodium sulfate, filtered, and concentrated. The residue was purified via Biotage (SNAP Cartridge KP Sil 25 g, 0-10% EtOAc/Hexane) to yield 5-bromo-N-[2-(methyloxy)ethyl]-2-nitroaniline (0.374 g, 1.286 mmol, 96 % yield). 1H NMR (400 MHz, CDCI3) delta 8.22 (br. s., 1 H), 8.04 (d, J = 9.1 Hz, 1 H), 7.05 (d, J = 1.5 Hz, 1 H), 6.78 (dd, 1 H), 3.69 (t, 2 H), 3.48 (t, 2 H), 3.45 (s, 3 H); MS (m/z) 275.1 (M+H)+.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; GLAXO GROUP LIMITED; BODMER, Vera, Q.; CASILLAS, Linda, N.; DEMARTINO, Michael, P.; KING, Bryan, W.; LAKDAWALA SHAH, Ami; LEISTER, Lara, Kathryn; WANG, Gren, Z.; WISNOSKI, David, Duff; HARRIS, Philip, A.; RAMANJULU, Joshi, M.; ROMANO, Joseph, J.; WILSON, Matthew, A.; WO2011/123609; (2011); A1;,
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