Morpholine, 4,4'-carbonylbis

110-91-8

32315-10-9

38952-62-4

GENERAL METHOD: To a solution of morpholine (5-10 eq.) in anhydrous dichloromethane (25 mL) was slowly added dropwise a solution of triphosgene (1 eq.) in anhydrous dichloromethane (5 mL) at 0°C. The reaction mixture was stirred continuously at 0°C for 1 hour, then warmed to room temperature and continued stirring for 4 hours. Upon completion of the reaction, water (100 mL) was added to dissolve the precipitate formed. The aqueous phase was extracted with dichloromethane (2 x 25 mL). The organic phases were combined and washed sequentially with 1N HCl (25 mL), saturated NaHCO3 solution (25 mL) and brine (25 mL). The organic layer was dried over anhydrous Na2SO4 and concentrated under reduced pressure to obtain dimorpholinomethyl ketone with purity >95%, which can be directly used in the subsequent reaction.