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We present the synthesis of high-purity polysarcosine (PSAR), a hydrophilic peptide derived from sarcosine that improves ADC pharmacokinetics and offers excellent biocompatibility. The solid phase peptide synthesis (SPPS) of Fmoc-Sar5-OH and modular synthesis of Fmoc-Sar10-OH and Ac-Sar10-OH are demonstrated, all with impurity levels below 0.1%. We also introduce a solid-phase strategy for peptide–oligonucleotide conjugates (POCs) using Boc/tBu side-chain protection and mild borate buffer deprotection to prevent oligonucleotide depurination and Arg deguanidation. This approach expands total stepwise synthesis for POCs. Finally, WuXi XDC’s capabilities in Antibody-Oligonucleotide Conjugate (AOC) services are highlighted.