Synthetic Route of 685115-77-9, 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 685115-77-9 as follows.
To a solution of 1-(3,5-dichloropyridin-4-yl)piperidine-4-carboxamide 23 (30 mg, 0.1 1 mmol) in THF (2 ml_), at 0 0C, was added a 1 M solution of borane THF complex in THF (11.1 ml_, 1.1 mmol). The reaction was stirred for 1 hour before warming to r.t. and stirring for a further 18 hr. To the reaction was added 2M HCI (2ml), the mixture diluted with water (20 ml) and extracted with EtOAc (2 x 20 ml.) and the combined organic extracts were washed with brine (25 ml_). The combined aqueous extracts were basified with saturated sodium hydrogen carbonate and then extracted with EtOAc (2 x 20 ml_). The combined organic extracts were washed with brine (20 ml_), dried (MgSO4) and concentrated under reduced pressure to give a crude colourless oil (8 mg). The crude product was purified by flash column chromatography on silica gel (CH2CI2, MeOH, 97:3 to CH2CI2, 1 M methanolic NH3, 9:1 ) to furnish the title compound, LC-MS (ESI, 3.5 min) R, 1.45 min, m/z 260 (91 %, [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,685115-77-9, its application will become more common.
Reference:
Patent; CANCER RESEARCH TECHNOLOGY LIMITED; McDONALD, Edward; BLAGG, Julian; PICHOWICZ, Mark; CRUMPLER, Simon Ross; WO2010/41054; (2010); A1;,
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