Arbeit komplett 12.07.2003 komplett Annahmeste - ArchiMeD

10 Experimenteller, chemisch-präparativer Teil 284
1 H-NMR δ [ppm]:
(300 MHz) Aceton-d6
13 C-NMR δ [ppm]:
(75 MHz) Aceton-d6
1.49 (t, 3 J=7.15, 3H, CH3, 2'''-H); 3.97 (s, 3H, CH3, 1'-H);
4.38 (s, 3H, CH3, N-CH3); 4.45 (q, 3 J=7.15, 2H, CH2, 1'''-H);
7.29 (dd, 3 J=9.54, 4 J=2.86, 1H, CH, 2-H); 7.33 (ddd,
3 J=7.39, 3 J=7.87, 4 J=0.95, 1H, CH, 8-H); 7.51 (ddd,
3 J=6.91, 3 J=7.15, 4 J=1.19, 1H, CH, 9-H); 7.70 (d, 3 J=8.35,
1H, CH, 10-H); 8.19 (d, 3 J=7.63, 1H, CH, 7-H); 8.79 (d,
3 J=9.30, 1H, CH, 1-H); 8.89 (d, 3 J=2.62, 1H, CH, 4-H); 9.01
(s, 1H, CH, 6-H)
13.71 (CH3, C-2'''); 33.36 (CH3, N-CH3); 54.40 (CH3, C-1');
59.94 (CH2, C-1'''); 106.74 (CH, C-4); 109.44 (CH, C-10);
115.63 (Cq, C-5); 116.22 (CH, C-2); 116.85 (2x Cq, C-4a,
C-6a); 117.22 (Cq, C-11b); 118.92 (CH, C-7); 120.12 (CH,
C-8); 122.93 (Cq, C-6b); 124.18 (CH, C-1); 124.79 (CH, C-
9); 125.21 (CH, C-6); 133.51 (Cq, C-11a); 141.12 (Cq, C-
10a); 157.75 (Cq, C-3); 167.22 (Cq, C-1'')
EI-MS (70 eV); m/z (%) 333.2 (_, 25.05), 262.0 (18.03), 149.3 (40.69), 138.0
(25.72), 120.3 (22.99), 107.0 (100.00), 92.4 (10.88), 77.3
(32.10), 43.9 (94.57)
Elementaranalyse (%): Ber.: C: 75.66 H: 5.74 N: 4.20
Gef.: C: 74.70 H: 6.04 N: 4.13
UV/VIS [nm]: lgε
CH2Cl2
λmax: 292.6 (5.74); λ1: 342.2 (5.13); λ2: 253.4 (5.44)
IR (KBr); ö [cm -1 ] 2963 (w) 2899 (w) 2859 (w) 2826 (w) 2765 (w)
2718 (w) 1700 (s) 1615 (s) 1574 (m) 1559 (w)
1516 (w) 1468 (s) 1436 (m) 1414 (w) 1391 (m)
1373 (s) 1330 (m) 1297 (m) 1284 (s) 1256 (s)
1246 (s) 1230 (s) 1217 (s) 1170 (s) 1156 (m)
1134 (s) 1072 (m) 1046 (m) 1027 (m) 992 (w)
979 (w) 919 (w) 881 (w) 858 (m) 842 (w)
822 (w) 810 (w) 780 (w) 742 (m) 732 (m)
675 (w)