Dissertation Martin Krause.pdf - KLUEDO - Universität Kaiserslautern

9c: Ausbeute: 118 mg (133 µmol, 89 % d.Th.)
Smp.: 55-65 °C.
20 19
O
18
17
16
O
O
3 2
11
5 6
7
O
10
9
8
O
12
4 1
O
O
1 H NMR (600 MHz, [D6]Aceton, 25°C)
δ = 1.20 – 1.24 + 1.25 – 1.36 + 1.39 – 1.47 + 1.62 – 1.64 (m, 12H, H-(19) + H-(20)), 1.71 – 1.74 +
1.92 – 1.90 (m, 8H, H-(18)), 2.39 – 2.43 (m, 2H, H-(17)), 3.65 – 3.68 (m, 16H, H-(14) + H-(15)), 3.82
– 3.83 (m, 8H, H-(13)), 4.00 – 4.03 + 4.07 – 4.09 (m, 8H, H-(12)), 6.77 (s, 2H, H-(5)), 6.90 (sbr, 4H,
H-(8) + H-(11)), 6.92 – 6.93 (m, 2H, H-(7)), 7.29 – 7.31 (m, 3H, H-(3) + H-(4)), 7.45 (sbr, 1H, H-(1)).
13C NMR (151 MHz, [D6]Aceton, 25°C)
δ = 25.0 (C-19), 25.1 (C-20), 25.5 (C-18), 42.8 (C-17), 68.8 + 68.9 + 69.0 (C-12), 69.3 (C-13), 70.4
(C-14), 71.0 (C-15), 75.7 (C-5), 112.8 (C-11), 113.4 (C-8), 119.7 (C-7), 124.2 + 124.3 (C-3), 125.7
(C-1), 125.8 (C-4), 128.3 (C-6), 133.5 (C-2), 141.4 (C-9), 148.9 + 149.0 (C-10), 173.7 (C-16).
MS (ESI TOF, positive mode): m/z (%): 913.4 (100 %) [M+Na + ], 929.3 (100%) [M+K + ].
IR (KBr, cm -1 ): 2930, 1734, 1508, 1458, 1262, 1129, 806.
Elementaranalyse: berechnet (%) für C50H66O14·H2O: C 66.06, H 7.54;
gefunden: C 66.30, H 7.25.
75
O
O
O
O
O
13
O
O
15
14