反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Synthesized as described for the preparation of compound BC1. Quantities: 25 (0.15 g, 0.25 mmol), 17 (0.11 g, 0.25 mmol), DMAP (0.03 g, 0.25 mmol), DCC (0.10 g, 0.5 mmol). Yield 0.18 g (72%). EA: Found: C, 69.39; H, 7.13. C58H69BrO10 requires C, 69.24; H, 6.91%. 1H NMR: δH (CDCl3; 300 MHz): 0.91 (3 H, t, 3J=6.8 Hz, CH3), 1.19-1.56 (34 H, m, CH2), 1.85 (6 H, m, O—CH2—CH2/Br—CH2—CH2), 3.43 (2 H, t, 3J=6.8 Hz, CH2Br), 4.08 (4 H, t, 3J=6.5 Hz, OCH2), 7.01 (2 H, d, 3J=8.8 Hz, Ar—H), 7.21 (3 H, m, Ar—H), 7.40 (4 H, d, 3J=8.6 Hz, Ar—H), 7.52 (1 H, t, 3J=8.1 Hz, Ar—H), 8.18 (4 H, d, 3J=8.8 Hz, Ar—H), 8.30 (4 H, d, 3J=8.6 Hz, Ar—H). 13C NMR: δC (CDCl3; 75 MHz): 14.5, 23.1, 26.4, 28.6, 29.2, 29.5, 29.75, 29.8, 29.85, 29.9, 29.95, 30.0, 32.3, 33.2, 34.4, 68.8, 114.7, 114.8, 116.2, 119.7, 121.4, 122.5, 127.0, 130.2, 132.2, 132.25, 132.3, 132.8, 151.8, 151.85, 155.9, 164.2, 164.5, 164.7. m/z (MALDI) 1028.00 (100%) and 1030.03 (97%) [M+Na]+, C58H69BrNaO10 requires 1027.40 (100%) and 1029.40 (97%).
WORKUP
后处理
- customSynthesized
- customas described for the preparation of compound BC1