Extraction method of tebuconazole intermediate ketene
An extraction method and a technology for ketene, which are applied in the field of extraction of tebuconazole intermediate ketene, can solve the problems of large environmental impact and difficulty in implementing a grinding method, improve the reaction yield and reduce connizzaro. Reaction, the effect of reducing side reaction products
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Embodiment 1
[0016] Tebuconazole intermediate enone extraction method:
[0017] The preparation method of pinacolone comprises: carry out the condensation reaction of chloropentane and formaldehyde under acidic conditions, catalyze with Zn / Co / Sb composite catalyst, the reaction temperature is 60 ℃, the reaction time is 4h, Zn / Co The ratio between the sum of the amount of substance of each component in the / Sb composite catalyst and the amount of substance of chloropentane is 3:50;
[0018] Using p-chlorobenzaldehyde and pinacolone as raw materials, add a composite catalyst and react in a methanol solvent system for 5 hours, the reaction temperature is 60°C, after the reaction is completed, the temperature is lowered to below 10°C, and the crystallized enone is filtered out. Wash with methanol, the mother liquor is applied mechanically for 5 times, the composite catalyst is a Zn / Co / Sb composite catalyst, and in the Zn / Co / Sb composite catalyst, the molar ratio of Zn:Co:Sb is 0.7:0.5:1.2 . ...
Embodiment 2
[0020] Tebuconazole intermediate enone extraction method:
[0021] The preparation method of pinacolone comprises: carry out condensation reaction under acidic condition by chloropentane and formaldehyde, carry out catalysis with Zn / Co / Sb composite catalyst, reaction temperature is 85 ℃, reaction time is 5h, Zn / Co The ratio between the sum of the amount of substance of each component in the / Sb composite catalyst and the amount of substance of chloropentane is 3:50;
[0022] Using p-chlorobenzaldehyde and pinacolone as raw materials, add a composite catalyst and react in a methanol solvent system for 5 hours, the reaction temperature is 60°C, after the reaction is completed, the temperature is lowered to below 10°C, and the crystallized enone is filtered out. Washing with methanol, the mother liquor is applied mechanically for 5 times, the composite catalyst is a Zn / Co / Sb composite catalyst, and in the Zn / Co / Sb composite catalyst, the molar ratio of Zn:Co:Sb is 1:0.7:1.2 .
Embodiment 3
[0024] Tebuconazole intermediate enone extraction method:
[0025] The preparation method of pinacolone comprises: carry out condensation reaction under acidic condition by chloropentane and formaldehyde, carry out catalysis with Zn / Co / Sb composite catalyst, reaction temperature is 95 ℃, reaction time is 5h, Zn / Co The ratio between the sum of the amount of substance of each component in the / Sb composite catalyst and the amount of substance of chloropentane is 3:50;
[0026] Using p-chlorobenzaldehyde and pinacolone as raw materials, add a composite catalyst and react in a methanol solvent system for 8 hours, the reaction temperature is 60°C, after the reaction is completed, the temperature is lowered to below 10°C, and the crystallized enone is filtered out. Washing with methanol, the mother liquor is applied mechanically for 5 times, the composite catalyst is a Zn / Co / Sb composite catalyst, and in the Zn / Co / Sb composite catalyst, the molar ratio of Zn:Co:Sb is 1.2:0.5:1 .
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