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. 33543-78-1, name is Ethyl 1H-imidazole-2-carboxylate, A new synthetic method of this compound is introduced below., Safety of Ethyl 1H-imidazole-2-carboxylate
tert-Butyl (2-bromoethyl)carbamate (17.59 g, 78.49 mmol) was added to ethyl 1H- imidazole-2-carboxylate (10 g, 71.36 mmol) and K2CO3 (11.83 g, 85.63 mmol) in DMF (200 mL) under nitrogen and the resulting mixture stirred at 80 C for 8 hours. The reaction mixture was diluted with EtOAc (300 mL), and washed sequentially with water (50 mL x 2). The aqueous layer was then further extracted with EtOAc (50 mL x 5). The combined organic phases were dried over MgS04, filtered and evaporated to afford crude product. The crude product was purified by flash silica chromatography, elution gradient 0 to 100% EtOAc in petroleum ether. Pure fractions were evaporated to dryness to afford ethyl 1 -(2-((tert-butoxycarbonyl)amino)ethyl)- lH-imidazole-2-carboxylate (Intermediate 7; 10.7 g, 53%) as a colourless liquid. 1HNMR (400 MHz, DMSO, 21 C) delta 1.20 (3H, t), 1.29 (9H, s), 3.26-3.34 (2H, m) 4.27 (2H, q) ,4.32-4.40 (2H, m), 6.90 (1H, s), 7.06 (1H, s), 7.32 (1H, s).
The synthetic route of 33543-78-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ASTRAZENECA AB; WARD, Richard, Andrew; JONES, Clifford, David; SWALLOW, Steven; GRAHAM, Mark, Andrew; DOBSON, Andrew, Hornby; MCCABE, James, Francis; (223 pag.)WO2017/80979; (2017); A1;,
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