Different variants of glutamate-urea-lysine-based PSMA-targeting ligands, varying in their linker moieties, were synthesized using solid phase chemistry, coupled to IRDye700DX, and labeled with 111In. A detailed description of the synthetic procedures and chemical analyses (HPLC, ESI-ion trap, MALDI-ToF) is provided in the supplemental information (Supplementary Materials and Methods and Results, Figure S1, Figure S2, Figure S8).All amino acids were purchased from Iris Biotech GmbH or Fluorochem unless stated otherwise. DOTA-NHS and DOTAGA anhydride were purchased from CheMatech SAS. IRDye700DX was purchased from LI-COR Biosciences. Other reagents were purchased from Fisher Scientific unless stated otherwise and were reagent grade. All water used was highly pure (18 mΩ) and all HPLC-grade solvents were purchased from Biosolve B.V. Identity of the peptides was confirmed using high-resolution mass spectra recorded on a JEOL AccuTOF (ESI-MS), and the dye-conjugated peptides with MALDI-ToF Mass spectrometry on a Bruker Microflex LRF MALDI-ToF.

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