Method for treating florfenicol fluorination process product
A treatment method and fluorination technology, which are applied in the field of treatment of florfenicol fluorination process products, can solve the problems of waste of fluorine elements, low utilization rate of fluorine elements, lack of treatment methods for florfenicol fluorination process products, etc. , to achieve the effect of improving economic value, high economic value and improving process efficiency
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Embodiment 1
[0024] (1) Reduction reaction: In the reaction kettle, add 201.20g of N,N-diethyl-2,3,3,3-tetrafluoropropionamide, the product of florfenicol fluorination process, add 1000g of methanol, and add Sodium 37.8g, add catalyst anhydrous zinc chloride 18.9g again. The reduction reaction was carried out at 30°C for 12 hours. After the reaction, rectification and recovery can be carried out directly to obtain 132.10 g of diethylamine product with a yield of 90.3%, and 122.8 g of 2,3,3,3-tetrafluoropropanol with a yield of 93%.
[0025] (2) Elimination reaction: 120 g of concentrated sulfuric acid was added to the 2,3,3,3-tetrafluoropropanol obtained in step (1), and the gas was collected by a gas collecting device. After reacting for 2 hours at a reaction temperature of 140° C., 100 g of the product 2,3,3,3-tetrafluoropropene can be prepared with a total yield of 87.7%.
[0026] The process can obtain diethylamine and 2,3,3,3-tetrafluoropropene, and has great economic value.
Embodiment 2
[0028] (1) Reduction reaction: In the reaction kettle, add 201.20 g of florfenicol fluorinated process product N,N-diethyl-2,3,3,3-tetrafluoropropionamide, add 500 g of ethanol, and add 460.3 g of formic acid g, add catalyst anhydrous aluminum trichloride 23.0g again. The reduction reaction was carried out at 80° C. for 3 hours. After the reaction, rectification and recovery can be carried out directly to obtain 135g of diethylamine product with a yield of 92.3%, and 124.8g of 2,3,3,3-tetrafluoropropanol with a yield of 94.5%.
[0029] (2) Elimination reaction: In the 2,3,3,3-tetrafluoropropanol obtained in step (1), add 14.2 g of phosphorus pentoxide, add 100 g of toluene, and carry out elimination reaction under strong stirring, using a gas collection device Collect gas. After reacting for 8 hours at a reaction temperature of 30° C., 103 g of the product 2,3,3,3-tetrafluoropropene can be prepared, with a total yield of 90.3%.
[0030] The process can obtain diethylamine a...
Embodiment 3
[0032] (1) Reduction reaction: In the reaction kettle, add 201.20g of N,N-diethyl-2,3,3,3-tetrafluoropropionamide, the product of florfenicol fluorination process, add 500g of methanol, and add Potassium 100g, then add catalyst anhydrous aluminum trichloride 10.0g. The reduction reaction was carried out at 70°C for 8 hours. After the reaction, rectification and recovery can be carried out directly to obtain 138g of diethylamine product with a yield of 94.3%, and 127g of 2,3,3,3-tetrafluoropropanol with a yield of 96.2%.
[0033] (2) Elimination reaction: In the 2,3,3,3-tetrafluoropropanol obtained in step (1), add 49 g of polyphosphoric acid, add 100 g of toluene, carry out the elimination reaction under strong stirring, and collect the gas by using a gas collection device . After reacting for 5 hours at a reaction temperature of 80° C., 108 g of the product 2,3,3,3-tetrafluoropropene can be prepared, with a total yield of 94.7%.
[0034] The process can obtain diethylamine...
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