Formic Acid → HCID 21430413, compound

Participants

Reaction Steps

A mixture of 2-(N-acetyl-2-ethoxyanilino)methylmorpholine hydrochloride (10 g.), formic acid (25 ml.) and formaldehyde (25 ml.; 40% solution) is heated at 95°-100° C. for 8 hours, poured onto ice (ca. 500 g.), basified (pH 11) with sodium hydroxide solution (40%) and extracted with ether (2× 200 ml.; 1× 100 ml.). The ethereal extracts are combined, dried (Na2SO4), filtered and the filtrate is treated with an excess of ethereal oxalic acid solution to give 2-(N-acetyl-2-ethoxyanilino)-4-methylmorpholine hydrogen oxalate, m.p. 186°-187° C. on recrystallisation from ethanol.

Provenance & Evidence