High-efficiency ionic liquid and cross-linked polystyrene-supported palladium catalyst and application thereof
A technology of ionic liquid and palladium catalyst, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, etc. It can solve the problem that does not meet the requirements of sustainable development and is difficult to recycle , environmental pollution and other issues, to achieve the effect of a wide range of reaction substrates, less catalyst consumption, and high reaction yields
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Embodiment 1
[0030] Synthesis of 3-(2,3-dihydroxypropyl)-1-vinylimidazolium chloride ionic liquid (1a)
[0031] Slowly add 11g (0.1mol) 1-chloro-2,3-dihydroxypropane dropwise into a 100mL round-bottomed flask containing 9.4g (0.1mol) 1-vinylimidazole, and slowly raise the temperature to 75°C. The reaction was continued for 48 hours. After the reaction, use diethyl ether (50mL×4) to wash off the unreacted raw materials, then use ethyl acetate (100mL×2) to extract the residue in the flask, and filter under reduced pressure to obtain a light yellow solid powder, which is obtained after vacuum drying Compound 1a (15.2 g, 74.5% yield). 1 H NMR (D 2 (0, 400MHz): δ8.997(s, 1H), 7.731(s, 1H), 7.532(s, 1H), 7.084(dd, J=7.6Hz, 4.4Hz, 1H), 5.743(dd, J=6.8 Hz, 1.2Hz, 1H), 5.364(dd, J=4.0Hz, 4.4Hz, 1H), 4.335~4.378(m, 1H), 4.145~4.202(m, 1H), 3.981~4.078(m, 1H), 3.557(d, J=2.4Hz, 2H); 13 C NMR (D 2 O, 100MHz) δ128.14, 123.47, 119.37, 109.59, 95.11, 69.69, 62.36, 52.06; MS-ESI: 169.1 [M-Cl] + , 3...
Embodiment 2
[0033] Synthesis of [3-(2,3-dihydroxypropyl)-1-vinylimidazolium chloride]-styrene copolymer (1b)
[0034]In a 100mL round bottom flask, dissolve 5.2g (0.05mol) of styrene and 1.02g (0.005mol) of compound 1a in 50mL of methanol, heat up to 80°C, add 90mg (1mol%) of azobisisobutyronitrile (AIBN ). After continuing to react for 72 hours, the reaction was terminated, and a large amount of solid powder was suspended in the reaction liquid at this time. After standing still, the upper layer of methanol was poured out, and the solid powder was extracted with stirring with ethanol (100 mL×4) to remove unpolymerized reactants. After pumping under reduced pressure, a light yellow solid powder was obtained, and compound 1b (5.8 g, yield 93.2%) was obtained after vacuum drying. Elemental analysis: N 1.06, C 87.34, H 7.37.
Embodiment 3
[0036] Preparation of [3-(2,3-dihydroxypropyl)-1-vinylimidazolium chloride]-styrene copolymer supported palladium catalyst (1c)
[0037] 1 g of compound 1b was added to 50 mL of H 2 PdCl 4 In an aqueous solution (0.01M), stir at room temperature for 72 hours, filter with suction, wash with water (20mL×2) and ethanol (20mL×3) successively, and filter with suction to obtain a yellow solid powder. Put this yellow solid powder in 20mL water, add 10mL NaBH under stirring 4 (185mg, 5mmol) aqueous solution, reacted at room temperature for 4 hours, then filtered with suction, washed with water (20mL×2), ethanol (20mL×3), and filtered with suction to obtain a gray solid powder, which was dried in vacuo to obtain catalyst 1c. The Pd content of catalyst 1c was determined by ICP-AES to be 0.96wt%.
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