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High ambipolar mobility emissive conjugated polymers (HAME‐CPs) are perfect candidates for organic optoelectronic devices, such as polymer light emitting transistors. However, due to intrinsic trade‐off relationship between high ambipolar mobility and strong solid‐state luminescence, the development of HAME‐CPs suffers from high structural and synthetic complexity. Herein, a universal design principle and simple synthetic approach for HAME‐CPs are developed. A series of simple non‐fused polymers composed of charge transfer units, π bridges and emissive units are synthesized via a two‐step microwave assisted C−H arylation and direct arylation polymerization protocol with high total yields up to 61 %. The synthetic protocol is verified valid among 7 monomers and 8 polymers. Most importantly, all 8 conjugated polymers have strong solid‐state emission with high photoluminescence quantum yields up to 24 %. Furthermore, 4 polymers exhibit high ambipolar field effect mobility up to 10−2 cm2 V−1 s−1, and can be used in multifunctional optoelectronic devices. This work opens a new avenue for developing HAME‐CPs by efficient synthesis and rational design. [ABSTRACT FROM AUTHOR]

n‐Type conjugated polymers (CPs) are crucial in the applications of organic electronics. Direct coupling of electron‐deficient C−H monomer via selective C−H activation, namely C−H/C−H oxidative direct arylation polycondensation (Oxi‐DArP), is an ideal approach toward such CPs. Herein, Oxi‐DArP is firstly adopted to synthesize a high‐performance n‐type CP using a newly developed monomer, i.e. 3,6‐di(thiazol‐5‐yl)‐diketopyrrolopyrrole (Tz‐5‐DPP). Tz‐5‐DPP based homopolymer PTz‐5‐DPP with a molecular weight of 22 kDa has been synthesized via Oxi‐DArP. After n‐doping, PTz‐5‐DPP films exhibited electric conductivity values up to 8 S cm−1 and power factors (PFs) up to 106 μW m−1 K−2. Notably, this PF value is the highest for n‐type polymer thermoelectric materials to date. The Oxi‐DArP synthesis and the excellent n‐type performance of the polymer make this work an important step toward the straightforward and sustainable preparation of high‐performance n‐type polymer semiconductors. [ABSTRACT FROM AUTHOR]