Ethanolamine → HCID 20375033, compound

Participants

Reaction Conditions

Reaction Steps

To a suspension of (4,6-dichloro-2-pyrimidinyl-thio)-acetic acid (2.390 g.) in anhydrous benzene (24 ml.), 1.27 ml. of oxalyl chloride in anhydrous benzene (6 ml.) was added at room temperature. The reaction mixture was heated, with agitation, to 40° C., for 30 minutes and held for another 10 minutes at 60° C. The solvent was evaporated under vacuum to give an oily residue, which was taken up again in anhydrous chloroform (50 ml.). The chloroform solution was added drop by drop to a solution of ethanolamine (1.1 ml.) in anhydrous chloroform (40 ml.) while the temperature was kept at about 15° C. The mixture was held at ambient temperature for 60 minutes and the separated solid was then filtered off. The filtrate was evaporated under vacuum to obtain a residue which was crystallised from ethyl acetate/hexane (1.5 g.), m.p. 95°-96° C.

Provenance & Evidence