Formic Acid → HCID 13881467, compound

Participants

Reaction Steps

A solution of 7.5 g (85 mmoles) of acetyl formate (a mixed anhydride of formic acid and acetic acid) in 30 ml of dry chloroform is added dropwise, at room temperature, to a solution of 5.0 g (17.0 mmoles) of 1,3-bis(2',6'-dimethylphenyl)-2-imino-imidazolidine, prepared as described in Method (a) of Example 1, in 50 ml of dry chloroform. The resulting mixture is stirred at 45° to 50° C. for 4 hours, thereafter it is cooled with ice, and 10 ml of a 10% aqueous sodium hydrogencarbonate solution are added dropwise to the stirred mixture at a temperature not exceeding +10° C. The aqueous phase is separated, the chloroform phase is washed thrice with 50 ml of water each, dried over anhydrous sodium sulfate, filtered, and the solvent is evaporated under reduced pressure, 4.6 g (84.2%) of 1,3-bis(2',6'-dimethylphenyl)-2-formylimino-imidazolidine are obtained; the product melts at 306°-308° C. after recrystallization from methanol.

Provenance & Evidence