Extracurricular laboratory: Synthetic route of 490-11-9

According to the analysis of related databases, 490-11-9, the application of this compound in the production field has become more and more popular.

Reference of 490-11-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 490-11-9, name is Pyridine-3,4-dicarboxylicacid, molecular formula is C7H5NO4, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

10265] WXO18-1 (40.00 g, 239.35 mmol, 1.00 eq) was dissolved in anhydrous methanol (1.00 L), then concentrated sulfuric acid (11.98 g, 119.67 mmol, 6.51 mE, 98% purity, 0.50 eq) was added at 85 C. The mixture was stirred under nitrogen condition for 40 h. After reaction, the reaction liquid was concentrated under vacuum, then the concentrated solution was slowly added to saturated sodium bicarbonate solution (1,500 mE). The resulting mixture was stirred until there was no bubble generated, and extracted with ethyl acetate (1,000 mLx3). The organic phase was washed with saturated sodium chloride solution (800 mLx3), dried with anhydrous sodium sulfate and filtered. The filtrate was dried by rotary evaporation to obtain the brown oily compound WXO18-2. ?H NMR (400 MHz, CDC13) oe ppm: 9.06 (s, 1H), 8.82 (d, J4.90 Hz, 1H), 7.49 (d, J5.02 Hz, 1H), 3.94 (m, 6H).

According to the analysis of related databases, 490-11-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SHENZHEN SALUBRIS PHARM CO LTD.; Wu, Chengde; Yan, Jie; Xu, Wenjie; Yu, Tao; Li, Ning; Chen, Shuhui; US2018/305346; (2018); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem