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 100-26-5 as follows., 100-26-5
10311] Thionyl chloride (2.2 mE) was added dropwise to MeOH (14 mE) while stirring on ice. 2,5-Pyridinedicarbox- ylic acid (1.0 g, 6.0 mmoles) was added and the reaction heated at reflux for 3 hr. The reaction was cooled and the solvent removed under reduced pressure. The resulting residue was dissolved in DCM (15 mE), afier which saturated Na2CO3 (15 mE) was added while stirring on ice. Theaqueous layer was extracted with DCM (3x 15 mE), and the combined organics were washed with saturated Na2CO3 (2×40 mE), dried over Na2SO4(s), and concentrated under reduced pressure to afford the title compound (915 mg, 78%) as a pale yellow solid. ?H NMR (500 MHz, CDC13) oe 9.32 (dd, J=0.5, 2.0 Hz, 1H), 8.47 (dd, J=2.0, 8.0 Hz, 1H), 8.23 (dd, J=0.5, 8.0 Hz, 1H), 4.06 (s, 3H), 4.01 (s, 3H); ?3C NMR (125 MHz, CDC13) oe 165.0, 164.9, 150.8, 150.8, 138.4, 128.6, 124.7, 53.3, 52.8; HRMS (ESI) mlz 196.0600 [calc?d for C9H,QNO4 (M+H) 196.0605].
The chemical industry reduces the impact on the environment during synthesis 100-26-5, I believe this compound will play a more active role in future production and life.
Reference:
Patent; WISCONSIN ALUMNI RESEARCH FOUNDATION; RAINES, Ronald T.; Vasta, James; (50 pag.)US2016/280701; (2016); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem