Using the general previously reported method above, the 5-nitroisophthalic acid starting material (0.44550 g) was suspended in CH2Cl2 (25 mL), and oxalyl chloride (0.87 mL, ~2.2 equivs.) was added before the reaction mixture was heated to reflux where the reaction proceeded quickly. The associated colour change for the nitro intermediate was a bright translucent yellow solution of the desired product, which was isolated as a bright yellow crystalline solid in a yield of 0.5234 g (100%). The reaction flask containing the 5-nitroisophthaloyl dichloride (0.52340 g) was evacuated and charged with dry N2(g). The predried TBACl (2.93252 g, 5 equivs.) was pre-dissolved in CH2Cl2 (20 mL). The CH2Cl2:TBACl solution (10 mL) was added directly to the reaction flask and allowed to stir for 10 min. The ortho-phenylenediamine (0.25087 g, 1.1 equivs.) was pre-dissolved in the CH2Cl2:TBACl solution (10 mL) and then added to the reaction mixture over 2 min. After 10 min, the crude product was precipitated by adding CH3OH (40 mL). The precipitate was separated and washed with H2O (excess) and n-hexane (4×10 mL) to remove residual diamine. The crude was allowed to dry in the glass frit before being dissolved in a mixture of CH2Cl2 (40 °C, 15 mL) and TBACl (excess). The triturated mixture was placed in the freezer for 12 h, and the fine pale-yellow solid was separated and washed again with water (excess) and n-hexane (4×10 mL). The solid was collected, and anion exchange was then performed by suspending the solid in CH3CN (150 mL), KPF6 (10 equivs.) was added, and the mixture was stirred for 12 h. The fine light-yellow solid of 1a was filtered and washed with H2O (excess) before being dried in vacuo, with a final yield of 0.11261 g (9%).