This paper reports the resolution of racemic gossypol to optically active enantiomery by condensationof (±) gossypol with S-1-methylphenethylamine, followed by subsequent actetylation and hydrolysis. Sev-en isomers of hexaacetate of di-S-1-methylphenet-thylamino gossypol have been obtained by chromatog-raphy on silica gel, and also structures of the acetates have been determined. This paper reports the resolution of racemic gossypol to optically active enantiomery by condensation of (±) gossypol with S-1-methylphenethylamine, followed by subsequent actetylation and hydrolysis. Sev-en isomers of hexaacetate of di-S-1-methylphenet-thylamino gossypol have has obtained by chromatog-raphy on silica gel, and also structures of the acetates have been determined.