A composite catalyst for synthesizing tetrahydrofuran-3-carbaldehyde and method for using it to synthesize tetrahydrofuran-3-carbaldehyde
A composite catalyst, tetrahydrofuran technology, applied in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, physical/chemical process catalysts, etc. expensive effect
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Embodiment 1
[0021] 150g of 2,5-dihydrofuran was added to a 1L autoclave, 308g of tetrahydrofuran (with a water content of 0.1%) was added, and the catalyst HCCo 3 (CO) 9 1.5g, Fe(CO) 5 1.5g and 12g of tetrabutylammonium chloride, after passing through hydrogen to replace the air in the reactor, then passing through hydrogen at 0.5MPa, carbon monoxide at 0.5MPa, heating to 60°C, and reacting for 50h. After the reaction, the solvent tetrahydrofuran was evaporated under normal pressure for recycling, and then the product tetrahydrofuran-3-carbaldehyde was distilled under reduced pressure, with a purity of 98% and a yield of 90.6%. The remaining catalyst is recovered and applied mechanically.
Embodiment 2
[0023] Add 150 g of 2,5-dihydrofuran into a 1L autoclave, add 308 g of tetrahydrofuran (the mass fraction of water is 0.3%), and add the catalyst HCCo 3 (CO) 9 12g, Fe(CO) 5 9g and 1.5g of tetrabutylammonium chloride, after passing through hydrogen to replace the air in the reactor, then passing through hydrogen at 2.0MPa, carbon monoxide at 4.0MPa, heating to 120°C, and reacting for 3h. After the reaction, the solvent tetrahydrofuran was distilled off under normal pressure for recycling, and then the product tetrahydrofuran-3-carbaldehyde was distilled under reduced pressure, with a purity of 98% and a yield of 89.2%. The remaining catalyst is recovered and applied mechanically.
Embodiment 3
[0025] Add 150 g of 2,5-dihydrofuran and 1,508 g of methyl tert-butyl ether (the mass fraction of water is 0.1%) into a 2L autoclave, and add the catalyst ClCCo 3 (CO) 9 6g, Fe(OAc) 2 6g and 4.5g of dodecyltrimethylammonium chloride, after passing through hydrogen to replace the air in the kettle, then passing through hydrogen at 1.5MPa, carbon monoxide at 1.5MPa, heating to 80°C, and reacting for 40h. After the reaction was completed, the solvent methyl tert-butyl ether was distilled off under normal pressure for recycling, and then the product tetrahydrofuran-3-carbaldehyde was distilled out under reduced pressure, with a purity of 97% and a yield of 93.3%. The remaining catalyst is recovered and applied mechanically.
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