Chen Yu-yan
2004
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Journal
Fine chemicals
Abstract
2,6-Dimethoxypyridine(Ⅰ) was prepared from 2,6-dichlorpyridine firstly.Then by slow addition of bromine to Ⅰ at -20 ~ -40 ℃,3-bromo-2,6-dimethoxypyridine(Ⅱ) was produced in 74.8% yield.Electrophilic substitution of Ⅱ with Ph_2PCl at -78 ℃ gave 3-bromo-2,6-dimethoxy-4-diphenylphosphinopyridine(Ⅲ) in 77.4% yield.Finally,oxidation of trivalent phosphorous in Ⅲ at 0 ℃ and coupling reaction of the pyridine ring at 150 ℃ were used to synthesize the target product 2,2′6,6′-tetramethoxy-4,4′-diphenylphosphinoyl-3,3′-bipyridyl.The yields were 95.3% and 62.5% respectively.Structural analyses of the important intermediates and the target product were done by ~1HNMR and ~(13)CNMR.