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Analysis data for probe SAFit2 and controls ddSAFit2, 18(S)-Me


SAFit2


HRMS m/z = 803.4465 [M+H]+ (1.55 ppm errror)
UHPLC-MS tR = 1.614 min; purity: > 99 %
1H NMR (500 MHz, CDCl3, mixture of rotamers 0.35:1, A:B) δ 7.29 (t, J = 7.9 Hz, 0.27H, A), 7.09 (t, J = 7.9 Hz, 0.75H, B), 6.96 – 6.94 (m, 0.26H, A), 6.91 – 6.90 (m, 0.24H, A), 6.88 – 6.85 (m, 0.27H, A), 6.80 – 6.78 (m, 0.29H, A), 6.77 – 6.73 (m, 1.59H, A+B), 6.71 – 6.69 (m, 0.90H, B), 6.68 – 6.67 (m, 0.12H, A), 6.66 – 6.65 (m, 0.28H, A), 6.64 – 6.61 (m, 1.52H, A+B), 6.48 (s, 1.46H, A+B), 6.42 – 6.39 (m, 1.28H, A+B), 5.80 (dd, J = 6.2, 7.7 Hz, 0.25H, A), 5.56 (dd, J = 5.5, 8.2 Hz, 0.76H, B), 5.47 – 5.44 (m, 0.74H, A+B), 4.71 (d, J = 5.6 Hz, 0.24H, A), 4.55 (d, J = 13.6 Hz, 0.24H, A), 4.12 – 4.05 (m, 1.98H, A+B), 3.96 – 3.90 (m, 0.78H, B), 3.86 – 3.82 (m, 7.85H, A+B), 3.77 (s, 1.94H, A+B), 3.73 – 3.70 (m, 7.31H, A+B), 3.37 (d, J = 9.8 Hz, 0.68H, B), 2.98 (d, J = 9.7 Hz, 0.22H, A), 2.81 – 2.76 (m, 6.08H, A+B), 2.59 – 2.55 (m, 4.06H, A+B), 2.47 – 2.36 (m, 1.49H, A+B), 2.31 – 2.24 (m, 1.02H, A+B), 2.12 – 2.05 (m, 1.31H, A+B), 1.99 – 1.92 (m, 0.67H, B), 1.90 – 1.81 (m, 1.68H, A+B), 1.69 – 1.54 (m, 5.91H, A+B), 1.45 – 1.40 (m, 0.69H, B), 1.35 – 1.22 (m, 2.51H, A+B), 1.18 – 1.09 (m, 2.34H, A+B), 0.93 – 0.87 (m, 0.88H, B), 0.78 – 0.73 (m, 0.82H, B), 0.63 – 0.54 (m, 0.46H, A)
13C NMR (126 MHz, CDCl3, mixture of rotamers 1:3, A:B) δ 172.46 (B), 172.34 (A), 170.76 (A), 170.64 (B), 159.10 (A), 158.71 (B), 153.42 (A), 153.18 (B), 149.14 (A), 149.02 (B), 147.68 (A), 147.46 (B), 141.96 (B), 141.65 (A), 137.18 (A), 137.05 (B), 134.38 (A), 133.70 (B), 133.63 (B), 133.42 (A), 129.88 (A), 129.66 (B), 120.39 (B), 120.26 (A), 119.26 (A), 118.59 (B), 114.23 (A), 113.88 (B), 113.43 (A), 113.22 (B), 112.01 (B), 111.91 (A), 111.60 (A), 111.50 (B), 106.00 (B), 105.51 (A), 75.77 (B), 67.03 (B), 65.94 (A), 65.86 (B), 61.01 (A), 60.89 (B), 57.79 (B), 56.49 (A), 56.21 (B), 56.10 (A), 56.07 (B), 56.03 (A), 55.98 (B), 55.87 (A), 55.17 (B), 54.22 (B), 52.16 (B), 43.73 (B), 41.50 (B), 41.27 (A), 39.59 (A), 38.73 (B), 38.17 (B), 37.96 (A), 33.13 (A), 32.93 (B), 31.62 (A), 31.18 (B), 30.80 (B), 30.63 (A), 26.93 (B), 26.72 (B), 26.59 (A), 26.36 (B), 26.32 (B), 26.25 (A), 25.69 (B), 24.48 (A), 21.11 (B), 20.81 (A)


ddSAFit2


HRMS m/z = 803.4461 [M+H]+ (1.96 ppm errror)
UHPLC-MS tR = 1.881 min; purity: > 99 %
1H NMR (500 MHz, CDCl3, mixture of rotamers 0.36:1, A:B) δ 7.30 – 7.27 (m, 0.19H, A), 7.19 (t, J = 7.9 Hz, 0.70H, B), 6.97 – 6.93 (m, 0.25H, A), 6.91 – 6.88 (m, 0.26H, A), 6.88 – 6.85 (m, 0.24H, A), 6.81 – 6.73 (m, 3.24H, A+B), 6.70 – 6.65 (m, 0.55H, A), 6.61 – 6.56 (m, 1.49H, B), 6.50 (s, 1.47H, B), 6.42 (s, 0.53H, A), 5.79 (dd, J = 6.1, 7.8 Hz, 0.25H, A), 5.56 (dd, J = 5.2, 8.3 Hz, 0.72H, B), 5.43 – 5.40 (m, 0.70H, B), 4.74 (d, J = 5.5 Hz, 0.23H, A), 4.66 (d, J = 13.6 Hz, 0.25H, A), 4.14 – 4.03 (m, 2.54H, A+B), 3.99 – 3.94 (m, 0.73H, B), 3.87 – 3.81 (m, 8.91H, A+B), 3.77 (s, 6.21H, A+B), 3.74 – 3.71 (m, 3.92H, A+B), 3.39 (d, J = 9.7 Hz, 0.72H, B), 3.10 (d, J = 9.6 Hz, 0.27H, A), 3.02 – 2.93 (m, 1.10H, A+B), 2.87 (s, 0.35H, A), 2.82 – 2.76 (m, 3.47H, A+B), 2.60 – 2.55 (m, 4.21H, A+B), 2.51 – 2.45 (m, 0.71H, A+B), 2.41 – 2.34 (m, 0.67H, B), 2.30 – 2.24 (m, 0.90H, A+B), 2.13 – 2.06 (m, 1.07H, A+B), 1.97 – 1.85 (m, 2.31H, A+B), 1.72 – 1.57 (m, 5.00H, A+B), 1.36 – 1.29 (m, 1.56H, A+B), 1.21 – 1.10 (m, 2.50H, A+B), 1.05 – 1.00 (m, 0.42H, A), 0.97 – 0.88 (m, 0.77H, B), 0.80 – 0.72 (m, 0.89H, B), 0.69 – 0.61 (m, 0.26H, A)
13C NMR (126 MHz, CDCl3, mixture of rotamers 1:3, A:B) δ 172.83 (B), 171.98 (A), 170.64 (A), 170.53 (B), 159.06 (A), 158.86 (B), 153.45 (A), 153.12 (B), 149.16 (A), 149.04 (B), 147.67 (A), 147.48 (B), 142.38 (B), 141.36 (A), 137.19 (A), 137.02 (B), 133.66 (B), 133.43 (A), 129.84 (A), 129.70 (B), 120.35 (B), 120.27 (A), 119.36 (A), 118.58 (B), 114.19 (A), 113.91 (B), 113.67 (A), 112.76 (B), 111.98 (B), 111.90 (A), 111.58 (A), 111.53 (B), 106.02 (B), 105.50 (A), 75.74 (B), 67.03 (B), 66.01 (A), 65.92 (B), 61.02 (A), 60.87 (B), 57.79 (B), 56.49 (A), 56.24 (B), 56.08 (B), 56.03 (A), 56.00 (B), 55.86 (A), 55.20 (B), 54.27 (A), 54.22 (B), 52.32 (B), 43.78 (B), 41.62 (B), 41.25 (A), 39.77 (A), 38.74 (A), 38.27 (B), 38.00 (A), 33.29 (A), 32.91 (B), 31.67 (A), 31.33 (B), 30.85 (B), 27.05 (A), 26.91 (B), 26.83 (A), 26.72 (B), 26.37 (B), 26.33 (B), 25.67 (B), 24.62 (A), 21.15 (A), 21.09 (B)


18(S)-Me


HRMS (ESI/QTOF) m/z = 498.1016 [M+H]+
HPLC Rt = 11.45 min
1H NMR (500 MHz, CDCl3) δ = 1.18 – 1.26 (m, 2H), 1.33 – 1.45 (m, 1H), 1.45 – 1.58 (m, 6H), 2.12 (tq,J = 12.9, 10.0, 8.5 Hz, 1H), 2.29 (dq, J = 14.8, 2.8, 2.4 Hz, 1H), 3.10 – 3.21 (m, 2H), 3.44 – 3.57 (m,2H), 3.89 (ddd, J = 6.7, 4.9, 1.9 Hz, 1H), 4.70 (dt, J = 6.0, 2.0 Hz, 1H), 6.07 (q, J = 6.9 Hz, 1H), 7.15(ddd, J = 7.8, 4.9, 1.1 Hz, 1H), 7.22 (d, J = 7.9 Hz, 1H), 7.47 (t, J = 1.8 Hz, 1H), 7.62 (dd, J = 7.4, 1.9Hz, 3H), 8.49 (ddd, J = 4.9, 1.9, 0.9 Hz, 1H)
13C NMR (126 MHz, CDCl3) δ = 15.1, 15.6, 28.2, 28.3, 43.5, 47.7, 52.5, 55.1, 57.2, 63.6, 122.5, 123.0, 124.9, 132.7, 136.3, 137.1, 144.0, 148.6, 158.9, 169.9