Acetonitrile → 1,1'-(Disulphanediyldiethane-2,1-diyl)bis(4-methylpyridinium)dibromide

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反応条件

反応手順

67 g of 4-picoline were diluted in 100 ml of acetonitrile and the mixture was brought to 80° C. A mixture of 60 g of 1-bromo-2-[(2-bromoethyl)disulphanyl]ethane and 15 ml of N-methylpyrrolidone (NMP) was added over 5 min. After stirring for 4 h at 85° C., the mixture was cooled. The solid obtained was filtered, rinsed with 3×200 ml of acetonitrile then dissolved in 800 ml of isopropanol (under reflux). After cooling, 1 l of ethyl ether was added. The precipitate formed was filtered, rinsed with 3×200 ml of ethyl ether, then dried. The off-white powder obtained (73.77 g) very predominantly contained (>90%) the expected product which was used as such for the following step.

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