反应详情

Salen ligand (C0) (1.0 g, 3.9 mmol) and aluminium triethoxide (1.2 g, 7.4 mmol) were dissolved in dry toluene (25 mL). The reaction mixture was refluxed for 4 hours after which the toluene was evaporated and the resulting yellow residue taken up in dichloromethane and washed with water (3×100 mL) and saturated brine (100 mL). After evaporation of the organic phase, a light yellow powder was obtained which was washed with diethyl ether (ca. 50 mL) and dried to give salen complex (C1) (1.2 g, 49%). 1H NMR 3.87 (8H, s, 2×CH2CH2), 6.7-6.9 (8H, m, 8×HAr), 7.1-7.3 (8H, m, 8×HAr), 8.29 (4H, s, 4×CHN). 13C NMR 60.14, 65.09, 117.36, 119.00, 131.81, 132.74, 161.46, 166.85. m/z (ESI) Found: 603.1775 C32H25N4O5Al2 (MH+), Requires 603.1769.

1. customwas evaporated
2. washwashed with water (3×100 mL) and saturated brine (100 mL)
3. customAfter evaporation of the organic phase
4. customa light yellow powder was obtained which
5. washwas washed with diethyl ether (ca. 50 mL)
6. customdried