The alkaloids of ipecacuanha have been fractionated by countercurrent distribution. A simple method for the isolation of all previously known non-phenolic alkaloids has been developed and two new alkaloids (protoemetine and ipecac-alkaloid A) have been isolated. The infrared spectrum of O-methylpsychotrine has been compared with the spectra of model compounds; it is thereby confirmed that the double bond in this alkaloid is endocyclic.