To a solution of TBTQ 1 (20 mg, 0.043 mmol) and 2,5-dimethoxy-terephthaldehyde 3 (12.6 mg, 0.0649 mmol) in deuterated chloroform (4 ml) in a screw-capped 8 ml glass vial, a catalytic amount of TFA (0.4 µl, 0.0052 mmol) was added and the reaction mixture was stirred at r.t. for 3 days. Afterwards, the crude reaction mixture was washed with aqueous K2CO3 solution (0.25 M, 3 × 2 ml), dried over Na2SO4 and concentrated under reduced pressure. The resulting red solid was immediately dissolved in DCM and purified by r-GPC (DCM, 30 °C, 5 ml min−1) to give 14 mg (46%) of (OMe-cube)2 as a yellow solid. Melting point, 315 °C (decomposed). 1H NMR (600 MHz, CD2Cl2): δ (ppm) = 8.90 (s, 6H, HC=N), 8.87 (s, 6H, HC=N), 8.85 (s, 12H, HC=N), 8.82 (s, 6H, HC=N), 8.78 (s, 6H, HC=N), 8.65 (s, 6H, HC=N), 8.38 (s, 6H, HC=N), 8.03 (s, 6H, Ar–H), 7.88 (s, 6H, Ar–H), 7.79 (s, 6H, Ar–H), 7.71 (s, 6H, Ar–H), 7.69 (12H, Ar–H), 7.53 (d, 3J = 8.4 Hz, 6H, TBTQ Ar–H), 7.41 (d, 3J = 8.4 Hz, 6H, TBTQ Ar–H), 7.38 (d, 3J = 8.4 Hz, 6H, TBTQ Ar–H), 7.36–7.32 (m, 6H, TBTQ–Ar–H and Ar–H), 7.27 (s, 6H, TBTQ–Ar–H), 7.24 (s, 12H, Ar–H, TBTQ–Ar–H), 7.21 (s, 6H, TBTQ–Ar–H), 7.19 (s, 6H, TBTQ Ar–H), 7.17–7.14 (m, 6H, TBTQ–Ar–H), 7.08 (d, 3J = 8.4 Hz, 6H, TBTQ–Ar–H), 7.03–6.97 (m, 18H, TBTQ–Ar–H), 6.89 (s, 6H, TBTQ–Ar–H), 6.83 (d, 3J = 8.4 Hz, 6H, TBTQ–Ar–H), 6.78 (d, 3J = 8.4 Hz, 6H, TBTQ–Ar–H), 6.77 (d, 3J = 8.4 Hz, 6H, TBTQ–Ar–H), 6.72 (s, 6H, TBTQ–Ar–H), 6.59 (d, 3J = 8.4 Hz, 12H, TBTQ–Ar–H), 6.26 (d, 3J = 7.8 Hz, 6H, TBTQ–Ar–H), 4.04 (s, 18H, OCH3), 3.94 (s, 18H, OCH3), 3.90 (s, 18H, OCH3), 3.86 (s, 18H, OCH3), 3.82 (s, 18H, OCH3), 3.67 (s, 18H, OCH3), 3.11 (s, 18H, OCH3), 2.85 (s, 18H, OCH3), 2.30–1.74 (m, 96H, –CH2CH2CH3) 1.71 (s, 30H), 1.64 (s, 18H), 1.35–1.09 (m, 84H, –CH2CH2CH3), 1.0–0.90 (m, 126H, –CH2CH2CH3), 0.77–0.72 (m, 12H, –CH2CH2CH3), 0.48 (t, 3J = 7.2 Hz, 18H, –CH2CH2CH3). 13C NMR (151 MHz, CD2Cl2): δ (ppm) = 156.5, 155.7, 155.3, 155.2, 155.0, 154.6, 154.31, 154.26, 154.2, 153.9, 153.8, 153.1, 152.7, 152.5, 152.6, 152.3, 152.2, 150.1, 149.8, 149.64, 149.6, 149.5, 149.4, 149.3, 149.1, 146.7, 146.6, 146.4, 146.1, 146.0, 145.5, 145.4, 129.0, 128.9, 128.6, 128.55, 128.49, 127.8, 125.0, 124.6, 124.42, 124.36, 124.2, 124.0, 119.8, 119.7, 119.4, 119.04, 118.96, 118.8, 118.5, 118.4, 118.1, 117.5, 117.3, 116.1, 116.0, 111.2, 110.2, 109.83, 109.77, 109.63, 109.58, 73.5, 73.2, 73.0, 67.39, 67.35, 67.33, 67.23, 67.18, 66.9, 56.71, 56.68, 56.65, 56.61, 56.6, 56.4, 56.1, 55.4, 41.8, 41.2, 41.1, 41.0, 21.3, 21.1, 21.0, 20.9, 20.8, 20.3, 15.5, 15.4, 15.32, 15.29, 15.0, 14.9. Fourier transform infrared spectroscopy (neat, attenuated total reflectance): ?̃ (cm−1) = 2,999 (w), 2,957 (m), 2,925 (m), 2,870 (m), 2,853 (m), 1,734 (w), 1,616 (m), 1,593 (m), 1,492 (s), 1,482 (s), 1,465 (s), 1,410 (s), 1,373 (m), 1,211 (s), 1,140 (m), 1,043 (s), 974 (w), 882 (m), 821 (m), 701 (w). Ultraviolet–visible spectroscopy (CH2Cl2): λmax (nm) = 296, 406. MALDI–TOF (trans-2-[3-(4-tert-butylphenyl)-2-methyl-2-propenylidene]malononitrile (DCTB)): m/z [M]+ calculated for C752H768N48O48, 11,245.94; found, 11,245.57. Elemental analysis: calculated for C752H768N48O48·33CH2Cl2, C 67.11, H 5.98, N 4.79; found C 66.94, H 5.91, N 4.86.