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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

Active Publication Date: 2019-09-13
瑞孚信湖北药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few treatment methods for florfenicol fluorinated process products, and the utilization rate of fluorine is low. The by-product N,N-diethyl-2,3,3,3-tetrafluoropropionamide is more than 1000 tons per year. , which not only causes waste of fluorine, but also brings huge environmental pressure to the production of enterprises
[0004] In summary, there is still a lack of more effective treatment methods for florfenicol fluorinated process products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention discloses a method for treating a florfenicol fluorination process product. The method comprises a reduction reaction and an elimination reaction. A reducing agent is adopted for the molecular structure of N,N-diethyl-2,3,3,3-tetrafluoropropionamide to carry out a direct reduction reaction, a special catalyst anhydrous zinc chloride or anhydrous aluminum chloride is added to obtain an unexpected effect, and the direct reduction is adopted to obtain diethylamine and 2,3,3,3-tetrafluoropropanol. The process product treatment method effectively recovers four fluorine atoms, and alsocan directly obtain diethylamine, so wastes are changed into valuables, and the economic values are greatly increased.

Description

technical field [0001] The invention belongs to the technical field of veterinary drug synthesis, and in particular relates to a treatment method for a florfenicol fluorinated process product. Background technique [0002] Florfenicol (Florfenicol) Chinese name: fluprofen; Florfenicol is a commonly used veterinary antibiotic at present. It has a broad antibacterial spectrum, strong antibacterial effect, low minimum inhibitory concentration (MIC), and its antibacterial effect is 15-20 times that of chloramphenicol and thiamphenicol. At present, China is the main producer and exporter of veterinary antimicrobial Florfenicol. According to statistics, in 2015, the export of florfenicol in my country reached 2199 tons, and with the rectification of food safety in recent years, the amount used in the international animal protection market has continued to expand. [0003] The mainstream production process of florfenicol in China, the fluorination reaction uses Ishikawa reagent (...

Claims

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Application Information

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IPC IPC(8): C07C17/35C07C21/18C07C31/38C07C29/147C07C211/05C07C209/62
CPCC07C17/35C07C29/147C07C209/62C07C31/38C07C21/18C07C211/05
Inventor 张治国钟旭辉周国朝徐相雨
Owner 瑞孚信湖北药业有限公司