Reference of 113293-70-2, 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 113293-70-2 as follows.
NaH (613 mg, 15.4 mmol) was added portion wise to stirred anhydrous DMSO (10 mL). The mixture was heated to 80C until evolution of gas ceased and then cooled to 0C. A solution of (carbethoxymethyl)- triphenylphosphonium bromide (3.29 g, 7.74 mmol) in DMSO (5 mL) was then added and the mixture stirred at r.t for 30 min. The mixture was cooled to 0C and a solution of 2,6-dichloroisonicotinaldehyde (1 .35 g, 7.74 mmol) in DMSO (5 mL) was added and the mixture was stirred at r.t for 1 h. The mixture was then poured into aqueous 1 M HCI and extracted into DCM (3 x 50 mL). The organics were combined and washed with H2O (3 x 100 mL) and brine (2 x 100 mL), separated, dried (MgSO ) and concentrated. Purification by flash silica column chromatography (gradient elution /’-hex to 20% EtOAc in /-hex) gave the title compound as a yellow solid (1 .25 g, 66%). LCMS (ES+) 247 (M+H)+.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,113293-70-2, its application will become more common.
Reference:
Patent; CHDI FOUNDATION, INC.; LUCKHURST, Christopher A.; HAUGHAN, Alan F.; BRECCIA, Perla; STOTT, Andrew J.; BURLI, Roland W.; HUGHES, Samantha J.; MUNOZ-SANJUAN, Ignacio; DOMINGUEZ, Celia; MANGETTE, John E.; WO2012/103008; (2012); A1;,
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