Reference of 116855-08-4, 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 116855-08-4 as follows.
Step 5: lH-Pyrazolor3,4blpyridine-3-carboxylic Acid Methyl Ester The mixture of solids from the preceding step 4 (95 g) was suspended in methanol (500 mL) and sulfuric acid (5 mL) was added carefully. The reaction mixture was then heated to reflux for 6-8 h, and the reaction was monitored using TLC. After completion of the reaction, inorganic solids were filtered off from the reaction mixture and the solid cake was washed with hot methanol. The main filtrate and the washings were combined, then methanol was distilled off under reduced pressure on the rotary evaporator. The resulting solids were suspended in 5% sodium bicarbonate solution (300 mL) and stirred for 5 min. at room temperature. The white solids were filtered off and dried in an oven at 90-95 0C to constant weight (8.07 g, 42% based on 3-methyl-lH-pyrazolo[3,4b]pyridine), mp 201-203 0C. 1H NMR: (CDCl3) 14.4 (brs, 1 H), 8.74 (dd, J = 4.6 and 1.5 Hz, 1 H), 8.64 (dd, J = 8.1 and 1.5 Hz, 1 H), 7.39 (dd J = 8.1 and 4.6 Hz, 1 H), 4.10 (s, 3 H).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,116855-08-4, its application will become more common.
Reference:
Patent; UNIVERSITY OF KANSAS; GEORGE, Ingrid, Gunda; TASH, Joseph, S.; CHAKRSALI, Ramappa; JAKKARAJ, Sudhakar, R.; CALVET, James, P.; WO2011/5759; (2011); A2;,
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