Use of metal complex compounds as oxidation catalysts
A technology of metal complexes and compounds, applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, detergent complexing agents, etc., can solve problems such as dye and fiber damage
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Embodiment 1
[0584] Example 1 : Ethyl 4-chloropyridine-2-carboxylate
[0585]
[0586] a) Step 1:
[0587] At 40°C, 10.0ml (0.130mol) of N,N-dimethylformamide was added dropwise to 295ml (4.06mol) of thionyl chloride with stirring. Then, within half an hour, 100 g (0.812 mol) of picolinic acid were added. The mixture was carefully heated to 70°C and stirred at this temperature for 24 hours, the gas formed being conveyed away through a washing bottle containing sodium hydroxide solution. Concentration, co-evaporation with 100 ml of toluene each time, three co-evaporations; the product is diluted to 440 ml with this solvent, and the solution is introduced into a mixture of 120 ml of absolute ethanol and 120 ml of toluene. The mixture was concentrated to about half the volume, cooled to 4° C., filtered with suction and washed with toluene. This gives ethyl 4-chloropyridine-2-carboxylate hydrochloride in the form of a beige hygroscopic powder.
[0588] b) Step 2:
[0589] The hydroch...
Embodiment 2
[0591] Example 2 : Ethyl 3-(4-chloropyridin-2-yl)-3-oxopropionate
[0592]
[0593] Under a nitrogen atmosphere, 4 g (about 60% dispersion in paraffin oil, about 100 mmol) of sodium hydride were washed twice with 60 ml of n-hexane each time, and then 400 ml of anhydrous tetrahydrofuran were added. The mixture was heated to 50° C., and within 2 hours, a solution of 13.36 g (72 mmol) of ethyl 4-chloropyridine-2-carboxylate and 10.04 g (114 mmol) of ethyl acetate in 60 ml of anhydrous tetrahydrofuran was added dropwise thereto. During this time, the mixture began to boil vigorously. When the exothermic reaction subsided, it was stirred at room temperature for 12 hours to complete the reaction. The yellow suspension was poured into 400 ml of ice-water, neutralized with 15% hydrochloric acid, and the solution was concentrated to half its volume. It was then extracted twice with 200 ml each of ethyl acetate and the organic extracts were combined, dried (sodium sulfate), filte...
Embodiment 3
[0595] Example 3 : 6-(4-chloropyridin-2-yl)-2-pyridin-2-yl-pyrimidin-4-ol (ligand PM1)
[0596]
[0597] 13.15g (58mmol) of 3-(4-chloropyridin-2-yl)-3-oxopropionic acid ethyl ester was dissolved in 400ml of ethanol, followed by the addition of 9.10g (58mmol) of 2-amidinopyridine hydrochloride . After adding 14.44ml of 4N sodium hydroxide solution, it was refluxed for 7 hours. The mixture was cooled and concentrated to one-fifth of its original volume. The crude product was filtered and recrystallized from methanol to afford 6-(4-chloropyridin-2-yl)-2-pyridin-2-yl-pyrimidin-4-ol in the form of beige needles.
[0598] 1 H-NMR (360MHz, CDCl 3 ): 12.33 (br s, 1H); 8.76 (d, J=4.5Hz, 1H); 8.69 (d, J=5.4Hz, 1H); 8.62 (d, J=7.7Hz, 1H); 8.50 (d, J=1.8Hz, 1H); 8.15-8.03(tm, 1H); 7.75-7.63(m, 2H); 7.25(s, 1H).
PUM
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