Poly(hydroxystyrene) resins in which a portion of the hydroxyl groups are functionalized with t-butyloxycarbonyl groups ("t-Boc") tend to decompose during drying of the wet solid and on storage in the solid state. Solutions that are more stable than the solid material can be made from the wet freshly synthesized solid by dissolving the wet solid in a solvent that forms an azeotrope with water and then distilling the azeotrope of water and solvent from the solution until the solution contains less than about 1% by weight of water.