In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 114772-53-1 as follows. 114772-53-1
To a sealed tube were successively added TBAF 3H2O (0.35 g, 1.10 mmol), 4 (0.42 g, 2.20 mmol) and TMSN3 (0.38 g, 3.30 mmol) and the resulting mixture was heated at 120 C for 36 h. The resulting reaction mixture was extracted with EtOAc (30 mL) and TBAF was removed by washing the organic phase with 1 M HCl aqueous solution (3 10 mL). The organic extract was dried (Na2SO4), filtered and concentrated in vacuo. Recrystallization from diisopropyl ether furnished pure 5 (77%) as a white solid: M.p. 145-147 C; Rf 0.57 (CHCl3:MeOH, 9:1); tR 11.54 min (30% MeCN / 100% MeCN in 30 min); ESI-MS (m/z): 237.0 [MH]; 1HNMR(400 MHz, CD3OD): d 7.69-7.64 (m, 2H), 7.56-7.52 (m, 2H), 7.13 (d, 2H, J . 7.8 Hz), 7.00 (d, 2H, J . 7.8 Hz), 2.33 (s, 3H) ppm; 13C NMR (160 MHz, CD3OD): d 155.42, 142.17, 137.43, 136.24, 131.05, 130.39, 130.17, 128.76, 127.27, 122.83, 19.72 ppm.
According to the analysis of related databases, 114772-53-1, the application of this compound in the production field has become more and more popular.
Reference:
Article; Agelis, George; Resvani, Amalia; Matsoukas, John; Durdagi, Serdar; Spyridaki, Katerina; Liapakis, George; Tumova, Tereza; Slaninova, Jirina; Giannopoulos, Panagiotis; Mavromoustakos, Thomas; Vlahakos, Demetrios; European Journal of Medicinal Chemistry; vol. 55; (2012); p. 358 – 374,17;; ; Article; Agelis, George; Resvani, Amalia; Durdagi, Serdar; Spyridaki, Katerina; Tumova, Tereza; Slaninova, Jirina; Giannopoulos, Panagiotis; Vlahakos, Demetrios; Liapakis, George; Mavromoustakos, Thomas; Matsoukas, John; European Journal of Medicinal Chemistry; vol. 55; (2012); p. 358 – 374;,
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