Poly[2-(3-nitrocarbazolyl)ethyl methacrylate] (poly(NCzMA)) with controlled molecular weight and narrow molecular weight distribution was successfully synthesized using (methyl methacryloyl)potassium (MMA) as a weak initiator in the presence of diethylzinc (Et2Zn) in THF at -78 degreesC. Et2Zn acted both as an additive for the coordination with enolate anion and nino group and as a scavenger to remove impurities. Block copolymers PMMA-block-poly(NCzMA)-block-PMMA and poly(NCzMA)-block-PS-block-poly(NCz-MA). were also synthesized quantitatively (PMMA: poly(methyl methacrylate), PS: polystyrene). The results indicate that Et2Zn can be used to synthesize the polymers of solid, nitro group-containing methacrylate monomers by anionic polymerization of THF.