Living free radical polymerization was used to prepare poly(solketal methacrylate)-block-poly(2-(dimethylamino)ethyl methacrylate) or PSMA-b-PDMAEMA. A diblock with 105 SMA units and 122 DMAEMA units formed spherical micelles with PDMAEMA coronas and PSMA cores in water with 5 vol % THF. Nanospheres with cross-linked shells were obtained by cross-linking the PDMAEMA coronas with 1,2-bis(2'-iodoethoxyl)ethane (BIEE). The cores of the nanospheres were made hydrophilic by hydrolyzing the acetonide groups of PSMA.