Method for preparing unsaturated ketone from alkoxy propylene and propargyl alcohol
A technology of alkoxypropene and propargyl alcohol, which is applied in the field of producing VE main intermediates, to achieve the effects of reducing catalytic costs, improving catalytic efficiency, and reducing by-product formation
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Embodiment 1
[0048] First, 224.4 g (1 mol) of tetrahydro-dehydronerolidol, 204.2 g (2 mol) of acetic anhydride, and 1.4 g (0.01 mol) of methyl iodide were added to the autoclave. Seal the autoclave, and after confirming that the sealing is good, replace 6 times with nitrogen gas and 6 times with carbon monoxide gas with a hydrogen volume content of 1%, and press to an absolute pressure of 3.0 MPa. Turn on the stirring paddle and slowly add 72.1 g (1 mol) of methoxypropylene dropwise over 3 hours, keep the carbon monoxide pressure at an absolute pressure of 3.0 MPa, and keep the inner temperature of the reactor at 180° C. for 3 hours. After the stirring was stopped, the gas was discharged and the pressure was lowered to normal pressure, and a small amount of the reaction solution was taken for GC analysis.
[0049] Composition of the reaction liquid: 49.89% of tetrahydrofarnesone, 0.08% of tetrahydronerolidol, 38.51% of acetic anhydride, 11.37% of acetic acid, and 0.15% of others. The conv...
Embodiment 2
[0053] First, 154.1 g (1 mol) of dihydrodehydrolinalool, 20.4 g (0.2 mol) of acetic anhydride, and 2.1 g (0.015 mol) of methyl iodide were charged into the autoclave. Seal the autoclave, confirm that the sealing is good, replace 6 times with nitrogen and then 6 times with carbon monoxide gas with a hydrogen volume content of 2%, and press to an absolute pressure of 5.0 MPa. Turn on the stirring paddle and slowly add 79.2 g (1.1 mol) of methoxypropylene dropwise over 3 hours, keep the carbon monoxide pressure at 5.0 MPa absolute, and keep the inner temperature of the reactor at 220°C for 6 hours. After stopping the stirring and cooling down to normal pressure, a small amount of reaction solution was taken for GC analysis.
[0054] Composition of the reaction liquid: 67.85% of dehydrogeranone, 1.09% of dihydrodehydrolinalool, 7.21% of acetic anhydride, 21.31% of acetic acid, 2.38% of methoxypropylene, and 0.16% of others. The conversion rate of dihydrodehydrolinalool is 98.4%, ...
Embodiment 3
[0056] First, 154.1 g (1 mol) of dihydrodehydrolinalool, 51.1 g (0.5 mol) of acetic anhydride, and 4.2 g (0.03 mol) of methyl iodide were charged into the autoclave. Seal the autoclave, and after confirming that the sealing is good, replace 6 times with nitrogen and then 6 times with carbon monoxide gas with a hydrogen volume content of 0.5%, and press to an absolute pressure of 5.0 MPa. Turn on the stirring paddle and slowly add 79.2 g (1.1 mol) of methoxypropylene dropwise over 4 hours, keep the carbon monoxide pressure at 5.0 MPa absolute, and keep the inner temperature of the reactor at 200°C for 4 hours. After stopping stirring and cooling down to normal pressure, a small amount of reaction liquid was taken for GC analysis.
[0057] Composition of the reaction liquid: 62.01% of dehydrogeranone, 0.15% of dihydrodehydrolinalool, 16.27% of acetic anhydride, 19.16% of acetic acid, 1.85% of methoxypropylene, and 0.56% of others. The conversion rate of dihydrodehydrolinalool i...
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