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Analysis data for probe A-485 and control A-486


A-485




MS (ESI pos.) m/z = 537.1 ([M+H]+, calcd. 537.2)
1H-NMR (500 MHz, DMSO-d6, 300K) δ = 8.74 – 8.65 (m, 1H), 7.55 (d, 3J = 9.0 Hz, 1H), 7.38 (dd, J = 8.6, 5.4 Hz, 2H, rotamer B), 7.31 – 7.17 (m, 4H), 7.14 (t, 3J = 8.8 Hz, 1H, rotamer A), 6.10 – 6.04 (m, 1H), 5.46 – 5.36 (m, 1H, rotamer A), 5.12 – 5.03 (m, 1H, rotamer B), 5.01 – 4.89 (m, 1H), 4.85 (d, 2J = 16.5 Hz, 1H, rotamer B), 4.75 (d, 2J = 18.7 Hz, 1H, rotamer A), 4.62 – 4.50 (m, 1H), 4.44 (d, 2J = 16.5 Hz, 1H, rotamer B), 4.21 (d, 2J = 17.1 Hz, 1H, rotamer A), 3.18 – 3.06 (m, 1H), 3.05 – 2.93 (m, 1H), 2.69 – 2.58 (m, 4H), 2.54 – 2.43 (m, 1H), 1.38 (d, 3J = 6.6 Hz, 1H, rotamer B), 1.34 (d, 3J = 7.2 Hz, 1H, rotamer A); rotamer A> rotamer B (7:3)
13C-NMR (126 MHz, DMSO-d6, 300K) (mixture of rotamers) δ = 173.9, 173.8, 167.6, 161.4 (d, 1JCF = 243.1 Hz), 161.0 (d, 1JCF = 242.2 Hz), 155.6, 154.1, 154.0, 146.4, 146.3, 143.2, 134.0 (2x), 133.2 (2x), 129.6, 128.2 (d, 3JCF = 7.9 Hz), 127.8 (d, 3JCF = 8.2 Hz), 125.6 (d, 1JCF3 = 283.9 Hz) 124.3, 116.9, 115.6 (d, 2JCF = 21.5 Hz), 114.9 (d, 2JCF = 21.2 Hz), 113.3, 94.1, 94.0, 52.5 (q, 3JCF3 = 29.7 Hz), 50.03 (q, 3JCF3 = 30.6 Hz), 45.2, 44.9, 41.8, 41.4, 36.2, 34.9, 34.8, 29.8, 26.2, 24.3, 23.7, 12.3, 10.87
HPLC tR = 6.026 min; purity: ≥95%


A-486




1H-NMR (500 MHz, DMSO-d6, 300K) δ = 8.58 (s, 1H), 7.56 (dd, J = 8.3, 2.1 Hz, 1H, rotamer A), 7.51 (dd, J = 8.3, 2.1 Hz, 1H, rotamer B), 7.38 (dd, J = 8.5, 5.4 Hz, 2H rotamer B), 7.33–7.31 (m, 1H, rotamer B), 7.30–7.21 (m, 4H, rotamer A), 7.14 (t, 3J = 8.8 Hz, 1H, rotamer A), 6.03–5.94 (m, 1H), 5.45–5.35 (m, 1H, rotamer A), 5.09–5.03 (m, 1H, rotamer B), 4.97 (dd, J = 28.9, 17.9 Hz, 2H), 4.86 (d, 3J = 16.5 Hz, 1H, rotamer B), 4.75 (d, 3J = 18.7 Hz, 1H, rotamer A), 4.62–4.53 (m, 1H), 4.43 (d, 3J = 16.5 Hz, 1H, rotamer B), 4.22 (d, 3J = 17.1 Hz, 1H, rotamer A), 3.12–2.91 (m, 2H), 2.70–2.58 (m, 4H), 2.55–2.42 (m, 1H), 1.38 (d, 3J = 6.7 Hz, 3H, rotamer B), 1.34 (d, 3J = 7.2 Hz, 3H, rotamer A); rotamer A> rotamer B (7:3)
13C-NMR (126 MHz, DMSO-d6, 300K) (mixture of rotamers) δ = 173.6, 173.5, 167.4, 166.7, 161.4 (d, 1JCF = 243.1 Hz), 161.0 (d, 1JCF = 242.2 Hz), 155.7 (2x), 154.1, 154.0, 140.1 (2x), 137.4 (2x), 134.0 (2x), 133.2 (2x), 128.3 (d, 3JCF = 8.1 Hz), 127.8 (d, 3JCF = 8.3 Hz), 126.7 (q, 1JCF3 = 283.3 Hz), 125.3, 121.0 (2x), 115.6 (d, 2JCF = 21.5 Hz), 114.9 (d, 2JCF = 21.4 Hz), 112.7, 112.6, 94.0, 93.9, 52.5 (q, 2JCF3 = 29.2 Hz), 50.5 (q, 2JCF3 = 29.6 Hz), 45.1, 44.8, 41.8, 41.4, 35.4, 35.2, 29.0 (2x), 26.2 (2x), 14.1, 12.2, 10.9
MS (ESI pos.) m/z = 537.2 ([M+H]+, calcd. 537.2)
HPLC tR = 6.051 min; purity: ≥95% (Traces of DCM and EE)