With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.115754-62-6,((1,3-Dioxolan-2-yl)methyl)tributylphosphonium bromide,as a common compound, the synthetic route is as follows.
5.0 g (0.02548 mol) of 3,4,5-trimethoxy benzaldehyde and 33 ml of a 1M solution of previously made Wittig Salt III [4] in dimethylformamide (DMF) (1.3 equivalents, 0.03312 mol) was added to 150 ml 95% EtOH under N2 and warmed to dissolve all solids. 19 ml 2M NaOEt (1.5 equivalents, 0.03822 mol) was added drop-wise, and the reaction was heated to 60 C. for 48 hours. The mixture was poured into 300 ml H2O, extracted with 3¡Á75 ml EtOAc, washed with 2¡Á40 ml H2O and 2¡Á40 ml brine, dried with MgSO4, and concentrated by rotary evaporation. The resulting yellow solids were added to 150 ml THF. 100 ml 2M HCl was added to this solution and stirred for one hour at 20 C. Most of the solvent was removed by rotary evaporation, and the remainder was poured into 100 ml H2O. The product was extracted, washed, and dried as before, giving 5.2 g of impure yellow oil. This oil was purified through a short silica gel column, eluting with CH2Cl2 giving 4.02 g of a yellow solid, (E)-4-(3,4,5-trimethoxyphenyl)but-3-en-2-one intermediate product. The total yield was 4.02 g or 71%.1H NMR (500 MHz, CDCl3), delta 9.66 (d, J=8 Hz, 1H), 7.37 (d, J=16 Hz, 1H), 6.77 (s, 2H), 6.62 (dd, J=16 Hz, J=8 Hz, 1H), 3.88 (s, 9H), 115754-62-6
115754-62-6 ((1,3-Dioxolan-2-yl)methyl)tributylphosphonium bromide 22292430, acatalyst-ligand compound, is more and more widely used in various fields.
Reference£º
Patent; Spangler, Brenda D.; Spangler, Charles W.; Tarter, E. Scott; US2009/43109; (2009); A1;,
Metal catalyst and ligand design
Ligand Template Strategies for Catalyst Encapsulation – NCBI