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 462-08-8 as follows., 462-08-8
To a flame-dried 500 mL round-bottom flask purged with N2 was added 3- aminopyridine (10.0 g, 105 mmol) and THF (109 mL). NaHMDS (210 mL, 1.0 M solution in THF, 210 mmol) was added dropwise over 1 h and the resulting red solution was stirred for 30 min. Di-tert-butyl dicarbonate (24.3 mL, 105 mmol) was added dropwise over 2 min. After 19 h, the dark red solution was concentrated to 100 mL and H2O (1.0 L) was added. The mixture was extracted with EtOAc (3×500 mL). The combined organic layers were washed with brine, dried (MgSO4) and concentrated to give product (19.9 g, 102 mmol, 97%) as a brown solid: 1H NMR (CDCl3, 400 MHz) 8.46 (d, J = 2.5 Hz, 1 H), 8.31 (dd, J = 4.7, 1.4 Hz, 1 H), 8.00 (d, J = 6.7 Hz, 1 H), 7.26 (dd, J = 8.4, 4.7 Hz, 1 H), 6.65-6.66 (m, 1 H) 1.55 (s, 9 H).
The chemical industry reduces the impact on the environment during synthesis 462-08-8, I believe this compound will play a more active role in future production and life.
Reference:
Patent; UNIVERSITY OF PITTSBURGH – OF THE COMMONWEALTH SYSTEM OF HIGHER EDUCATION; HURYN, Donna M.; WIPF, Peter; LAPORTE, Matthew G.; (137 pag.)WO2018/209083; (2018); A1;,
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