To explore the room‐temperature synthesis of metal phthalocyanines with unsaturated substituents, two zinc phthalocyanines with unsaturated alkoxy groups were synthesized in a reaction system composed of 4‐citronellol‐oxy‐phthalonitrile or 4‐geraniol‐oxy‐phthalonitrile, Zn(OAc)2⋅2H2O, DBU, and ethanol, at room temperature. The synthetic reactions lasted for 7 days and the yields of two phthalocyanine derivatives reached 21% and 18%, respectively, and they are inclined to protonation in a non‐coordinated organic solvent, for example, CHCl3. By the way, the phthalocyanine compounds with other metals, such as Cu, Ni, and Co, cannot be prepared. This work will provide preference for improving the synthetic method in the future, so as to synthesize many new phthalocyanine compounds in general laboratories.