“…Side‐chain liquid crystalline polypeptides bearing alkyl spacers (i.e., propyl, hexyl, and octyl), biphenyl mesogens, and oligo‐ethylene‐glycol tails (i.e., PPLG‐BPOEG m , PHLG‐BPOEG m , and POLG‐BPOEG m , m = 3 or 7) were synthesized by copper‐mediated alkyne‐azide 1,3‐dipolar cycloaddition between 4′‐prop‐2‐ynyloxy‐biphenyl‐terminated oligo‐ethylene‐glycols (PrBPOEG m , m = 3 or 7) and various poly( γ ‐azidopropyl/hexyl/octyl‐ l ‐glutamate)s (i.e., PAPLG, PAHLG, and PAOLG) (Scheme ). PrBPOEG m samples with different OEG length ( m = 3 or 7) were synthesized via two steps of etherifications from 4,4′‐dihydroxydiphenyl and OEG monomethylether . PAPLG 26 , PAHLG 34 , and PAOLG 32 with similar main‐chain lengths were prepared in four steps, including mono‐esterification of l ‐glutamic acid with chloropropyl/hexyl/octyl alcohols, cyclization of γ ‐chloropropyl/hexyl/octyl‐ l ‐glutamates, ring‐opening polymerizations, and nucleophilic substitution in the presence of sodium azide (NaN 3 ).…”