The chemical industry reduces the impact on the environment during synthesis 52133-67-2, name is Ethyl 2-cyano-4,4-diethoxybutyrate, I believe this compound will play a more active role in future production and life. 52133-67-2
To the 250 mL round bottomed flask containing 14.2 g (61.8 mmol) of ethyl 2,2-diethoxy cyanoacetate was added 110 mL of absolute ethanol followed by 28 mL of sodium ethoxide (21percent, 75.0 mmol). Thiourea (5.7 g, 74.5 mmol) was added all at once and the mixture was heated to 95¡ãC and refluxed overnight. The mixture was then cooled to room temperature and concentrated. Water (250 mL) was added and the aqueous layer was washed with diethyl ether (3 x 250 mL). The aqueous layer was then neutralized with acetic acid (1 eq.) and the precipitate was filtered. The yellow solid was dried under vacuum over P2O5 overnight to give 9.2 g (35.5 mmol, 57percent) of crude product. 1H-NMR (DMSO, 600 MHz): sigma 1.07 (t, 6H, J = 7.2 Hz), 2.43 (d, 2H, J = 5.4 Hz), 3.37 – 3.43 (m, 6H), 3.56 – 3.61 (m, 2H), 4.50 (t, 1H, J = 5.4 Hz), 6.07 (s, 2H), 11.5 (br s, 1H), 11.7 (br s, 1H). 13C-NMR (DMSO, 150 Mz): sigma 15.4, 27.9, 61.9, 85.7, 101.7, 151.9, 161.8, 172.9. HRMS (FAB): expected for C10H18N3O3S (M+H)+: 260.10634. Found: 260.10640. IR(neat): vmax 3342, 3219, 2973, 2879, 1563 cm-1.
The chemical industry reduces the impact on the environment during synthesis 52133-67-2. I believe this compound will play a more active role in future production and life.
Reference:
Article; Kim, Jiae; Wang, Ligong; Li, Yongfeng; Becnel, Kimberlynne D.; Frey, Kathleen M.; Garforth, Scott J.; Prasad, Vinayaka R.; Schinazi, Raymond F.; Liotta, Dennis C.; Anderson, Karen S.; Bioorganic and Medicinal Chemistry Letters; vol. 22; 12; (2012); p. 4064 – 4067;,
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