Scheme 1.

Synthesis of amphiphilic polyphenylene dendron conjugates. a) Benzophenone, toluene, and molecular sieves 4 Å, 15 h; b) TIPS‐acetylene, CuI, Pd(Ph₃P)₂Cl₂, THF/NEt₃ (5:1), RT, 15 h; c) TBAF, THF, 0 °C, 0.5 h; d) AB4 building block, o‐xylene, 160 °C, 24 h; c) TBAF, THF, 0 °C, 0.5 h; e) Surface building block, o‐xylene, 145 °C, 48 h; f) HCl, THF, 20 min; g) propargyl‐TEG‐COOH, EDC⋅HCl, DMAP, DMF, RT, 24 h; h) DMF, 180 °C, 36 h; i) RN₃, CuSO₄, sodium ascorbate, TBTA, DMF/H₂O (7:2 for 9a; 7:1 for 9b), RT, 24 h.