Provided are polymorphic forms of compound 5 or 5*, or mixtures thereof, and polymorph forms of compound 14 or 14*, or mixtures thereof. Also provided are methods of preparing compound 5 or 5*, or mixtures thereof, and methods of preparing compound of 14 or 14*, or mixtures thereof, which are useful as antifungal agents. In particular, provided is new methodology for preparing polymorphs of the compounds described and substituted derivatives thereof.