Synthetic Route of 77992-44-0, 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 77992-44-0 as follows.
A mixture of [5-BROMO-PYRIDINE-2-YL-HYDRAZINE] (4.34 g, 23.1 [MMOL)] and isobutyryl chloride (21.8 mL, 0.208 mol) is [REFLUXED] gently for 3 hours. The mixture is cooled to room temperature. Hexane (22.0 mL) is added and the slurry is stirred at room temperature for 15 minutes and filtered. The cake is washed with hexane (3x) and dried in a vacuum-oven (30- [35C)] for 48 hours. The product (5.90 [G,] yield 92.3%) is obtained as an off-white powder. A biphasic mixture of the product (5.87 [G,] 21.2 [MMOL),] water (12.0 mL) and dichloromethane (18.0 mL) is cooled to 5-10 [C.] A [1N] aqueous solution of [NAOH] (21.5 mL) is added over a period of 10 minutes. The mixture is stirred in the bath for 15 minutes. The organic layer is isolated and the aqueous layer extracted with dichloromethane (2x). The combined organic extracts are washed with 1: 1 brine-water and dried [(MGS04). MOST] of the dichloromethane is removed in vacuo. Ethyl acetate (8.0 mL) is added. After removing about half of the solvents, hexane is added. The slurry is stirred in an ice-water bath for 2 hours and filtered. The cake is washed with 9: 1 hexane-Ethyl acetate (3x) and dried in a vacuum-oven [(30-35C)] for 18 hours. The title compound may be obtained as a sandy tan powder (4.72g, 92.5%).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,77992-44-0, its application will become more common.
Reference:
Patent; PFIZER PRODUCTS INC.; WO2004/20440; (2004); A1;,
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