To achieve a concise "Shotgun" synthesis of GNRs, a key building block, that is 1,8-diaryl phenanthrene-2,7diboronic acid pinacol ester 3 was synthesized in three steps with gram scale (Scheme S2), which features with armchair and cove type edge (Scheme 1a). The introduction of sulfur to GNRs is achieved by the addition of 2,5dibromothiophene 2 as the functional block. In addition, 2substituted biphenyl 1 was introduced as the end block. Tert-butyl substituents were installed respectively on 1 and 3 to ensure the good solubility of the intermediates and the corresponding GNRs. With the key link block 3, functional block 2, and end block 1 in hand, a series of precursors of sulfur-doped AR-n were obtained and isolated through column chromatography in 53% (4a), 19% (4b), and 12% (4c) yield. By varying the end groups and adjusting the molar ratio of the three components, congeners with diverse lengths can be obtained (see Scheme S3 and Table for further details). The following ring-closing reactions of 4a and 4b by intramolecular oxidative cyclodehydrogenation in the presence of 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) and CF3SO3H gave the desired GNRs AR-11 and AR-17 in 95% and 93% yields, which were well-characterized by NMR analysis and HRMS. Due to the poor solubility of AR-23, well-resolved 1 H and 13 C NMR spectra could not be recorded. However, characterization was achieved by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) (Scheme 1c and Figure ). The Scholl reaction is conducted using superstoichiometric oxidants, limiting its scalability. To address these challenges, we also developed an electrochemical continuous flow Scholl reaction. This method eliminates the need for oxidants and enables the production of AR-11 in larger quantities. The arc lengths and arc-shaped of AR-11, AR-17 and AR-23 are 2.10 nm, 37.2° for AR-11, 3.29 nm, 51.4° for AR-17, and 4.49 nm, 70.6° for AR-23 based on density functional theory (DFT) optimized structures (Scheme 1a, Figure ). Source code of the program for the measurement of lengths and the arc-shaped was listed in Table . In addition, AR-11 and AR-17 were oxidized to give orange solid ARO-11 and ARO-17 with excessive meta-chloroperoxybenzoic acid (mCPBA) in 90% yields (Scheme 1b).