CN115703722A - Preparation method of N, N-dimethyl trifluoromethyl sulfonamide - Google Patents

Preparation method of N, N-dimethyl trifluoromethyl sulfonamide Download PDF

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CN115703722A
CN115703722A CN202110885160.9A CN202110885160A CN115703722A CN 115703722 A CN115703722 A CN 115703722A CN 202110885160 A CN202110885160 A CN 202110885160A CN 115703722 A CN115703722 A CN 115703722A
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dimethylamine
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dimethyltrifluoromethylsulfonamide
alcohol solvent
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施苏萍
汤涛
季宇轩
任齐都
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Jiangsu Guotai Super Power New Materials Co ltd
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Abstract

The invention discloses a preparation method of N, N-dimethyl trifluoromethyl sulfamide, which comprises the following steps: 1. dissolving dimethylamine in an alcohol solvent to form a dimethylamine alcohol solution, then adding trifluoromethyl sulfonyl halide, adding alkoxide corresponding to the alcohol solvent after complete reaction, and filtering and separating after complete reaction; distilling the filtrate under normal pressure to separate dimethylamine and alcohol solvent; 2. and distilling the filtrate, and rectifying and separating to obtain the N, N-dimethyl trifluoromethyl sulfonamide. The invention has the advantages that: the method solves the problems of decomposition and recovery of by-product dimethylamine hydrogen halide and recovery of alcohol solvents, obviously reduces the production cost, effectively improves the product purity, is easy to control the reaction, and is suitable for industrial production.

Description

Preparation method of N, N-dimethyl trifluoromethyl sulfonamide
Technical Field
The invention relates to the technical field of preparation of additives in lithium ion battery electrolyte, in particular to a preparation method of N, N-dimethyl trifluoromethyl sulfonamide.
Background
The lithium salt of sulfonamide and the additive thereof are widely researched and applied in the lithium battery electrolyte, and typical representative lithium salts are bis (trifluoromethyl) sulfonyl imide and lithium fluorosulfonimide. In addition, the derivatives of the additives, namely fluorosulfonyl isocyanate, N-dialkyl fluorosulfonamide and N, N-dialkyl trifluoromethanesulfonamide, are widely researched in the aspects of improving the high and low temperature storage performance and the flame retardant performance of the lithium ion battery. The N, N-dimethyl trifluoro sulfonamide not only can be used as an additive for improving the safety performance of the electrolyte, but also can be used as an additive for stabilizing more active electrochemical battery systems such as lithium sulfur, lithium oxygen, lithium metal and the like.
At present, the preparation methods of N, N-dimethyl trifluoromethyl sulfonamide mainly comprise the following two methods.
The first method comprises the following steps: according to patent application CN1289765A, dimethylamine gas is prepared by reacting dimethylamine hydrochloride and sodium hydroxide, the dimethylamine gas, gaseous trifluoromethyl sulfonyl fluoride and solvent ethyl ether are reacted at-78 ℃, and a product is obtained by washing, drying, evaporating the solvent and distilling the product.
And the second method comprises the following steps: see the literature (Russian Journal of General Chemistry, 2009, vol. 79, no. 2, pp. 315-322) which discloses the reaction of dimethylamine gas and trifluoromethanesulfonyl fluoride gas in an autoclave followed by extraction with ether, repeated washing of the by-products with ether followed by combined distillation, distillation of excess dimethylamine and ether and final distillation to give the product.
It can be seen that the basic principle of the above disclosed scheme is to prepare the product by reacting dimethylamine with trifluoromethanesulfonyl fluoride. However, in the industrial practical production, the technical scheme has the following problems: 1. the reaction by-product N, N-dimethyl hydrogen fluoride is not treated; 2. the reaction conditions are too harsh, which relates to ultralow temperature of-78 ℃, and the post-treatment is too complex, such as multiple extraction, water washing and other operations. The above problems can seriously affect the product quality, increase the production cost and are not beneficial to the industrialized implementation.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: the preparation method of the N, N-dimethyl trifluoromethyl sulfonamide has mild reaction conditions, is easy to separate and obtain products, solves the problems of treatment and recovery of byproducts, effectively reduces the production cost, and is easy to industrialize.
The applicant has conducted intensive studies on the above problems and combined with industrial experience, found the following methods: because dimethylamine has a high solubility in an alcohol solvent, the reaction can proceed in the forward direction by using an alcohol as a reaction solvent, dimethylamine as a reaction raw material, and an acid-binding agent. The reaction by-product N, N-dimethylhydrogen fluoride can dissociate dimethylamine and alcohol solvent under the action of alkaline substance, such as sodium methoxide, and then dimethylamine, alcohol solvent and product can be separated by subsequent purification operation, thereby obtaining N, N-dimethyltrifluoromethane sulfonamide and converting the by-product N, N-dimethylhydrogen fluoride into dimethylamine which is a reaction raw material, thereby completing the present invention.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a preparation method of N, N-dimethyl trifluoromethyl sulfamide comprises the following steps:
a preparation method of N, N-dimethyl trifluoromethyl sulfamide comprises the following steps:
1. dissolving dimethylamine in an alcohol solvent at the temperature of-15 to-30 ℃ to form dimethylamine alcohol solution, keeping the low temperature, and adding trifluoromethyl sulfonyl halide into the dimethylamine alcohol solution for reaction; adding alkoxide corresponding to the alcohol solvent after the reaction is completed, and filtering and separating after the reaction is finished to obtain filtrate and solid; the reaction equation is as follows:
Figure 214839DEST_PATH_IMAGE001
wherein X is selected from one of Cl and F, and M is selected from one of K, na and Ca;
2. distilling the filtrate at normal pressure to separate dimethylamine and alcohol solvent; then rectifying and separating to obtain the N, N-dimethyl trifluoromethyl sulfamide.
Further, in the above method for preparing N, N-dimethyltrifluoromethylsulfonamide, the alcoholic solvent in the first step is selected from one of methanol, ethanol, propanol and isopropanol.
Further, in the above method for preparing N, N-dimethyltrifluoromethylsulfonamide, the alkoxide in the first step is selected from a methoxide, an ethoxide, a propoxide, or an isopropoxide corresponding to the selected alcoholic solvent. The alkoxide corresponding to the solvent is selected, so that the solvent can be unified into one, the subsequent solvent separation is avoided, and the subsequent solvent recycling is facilitated.
Further, in the preparation method of the N, N-dimethyltrifluoromethylsulfonamide, methoxide is sodium methoxide, ethoxide is sodium ethoxide, propoxide is sodium propoxide, and isopropoxide is sodium isopropoxide.
Further, in the above method for preparing N, N-dimethyltrifluoromethanesulfonamide, the molar ratio of trifluoromethanesulfonyl halide, dimethylamine and alkoxide in the first step is 1:2:1 to 1:2.5:1. dimethylamine is used as a reaction raw material and also as an acid-binding agent in the reaction. Dimethylamine is in a slight excess state and can rapidly absorb acid generated in the reaction process.
Further, in the above method for preparing N, N-dimethyltrifluoromethylsulfonamide, the dimethylamine separated in the second step and the alcohol solvent are reused for the first step of the preparation process.
Further, the preparation method of the N, N-dimethyl trifluoromethyl sulfonamide is characterized in that the mass fraction of the dimethylamine alcohol solution formed in the first step is 10-20%.
Further, in the preparation method of the N, N-dimethyl trifluoromethyl sulfonamide, after the alkoxide is added in the first step, the reaction is carried out at a low temperature of-15 ℃ to-30 ℃, and then the reaction is finished after the temperature is raised to 0 ℃. The low-temperature reaction at the early stage can effectively reduce the occurrence of side reactions, and the subsequent heating can promote the complete reaction, thereby improving the product quality.
The invention has the advantages that: the alcohol reaction system is constructed, the reaction is easy to operate, the controllability is good, the two problems of decomposition of the byproduct dimethylamine hydrogen halide and recovery of the alcohol solvent are solved by adding alkoxide in the later period, the cost is greatly reduced, and the alcohol reaction system is suitable for industrial production and has high industrial utilization value.
Detailed Description
The preparation method of N, N-dimethyl trifluoromethyl sulfonamide according to the present invention is further described in detail with reference to the preferred embodiments.
The first embodiment is as follows: the reaction was carried out in a 2L four port glass jacketed kettle equipped with a coolant jacket, a stirrer, a thermometer, and a condenser, the coolant temperature was maintained at-30 ℃, 1014g of ethanol was added to the kettle, and 135g of dimethylamine was passed through the ethanol to obtain a dimethylamine ethanol solution. 228g of gaseous trifluoromethanesulfonyl fluoride was bubbled through the mixture with stirring and the reaction was maintained at-30 ℃ for 4 hours. Then 102g of sodium ethoxide is added, the mixture is stirred and reacts for 1 hour at the temperature of minus 30 ℃, the temperature is increased to 0 ℃, the reaction is continued for 2 hours, and the reaction is finished. The reaction mixture was sampled and examined for N, N-dimethyltrifluoromethanesulfonamide, and the yield was 98.2% based on trifluoromethanesulfonyl fluoride.
And filtering the reaction solution, distilling at normal pressure to obtain a mixed fraction, and detecting the contents of dimethylamine and ethanol in the fraction to obtain the recovery rates of the dimethylamine and the ethanol of 95.3 percent and 93.3 percent. And carrying out negative pressure rectification on the residual reaction liquid to obtain an N, N-dimethyl trifluoromethyl sulfonamide product with the purity of 99.6 percent.
Nuclear magnetic detection of the product: 1 H NMR(400 MHz,CDCl 3 ):δ 3.06（s,6H）；
19 F NMR(400 MHz,CDCl3): δ -75.1（s,3F）。
the second embodiment: the reaction was carried out in a 2L four-port glass jacketed kettle equipped with a coolant jacket, a stirrer, a thermometer, and a condenser, with the coolant temperature maintained at-30 ℃, 1014g of isopropanol was added to the kettle, and 135g of dimethylamine was passed through to obtain dimethylamine-isopropanol solution. 228g of gaseous trifluoromethanesulfonyl fluoride was passed through with stirring and the reaction was maintained at-30 ℃ for 5 hours. And then adding 123g of sodium isopropoxide, stirring and reacting at-30 ℃ for 1.5h, heating to 0 ℃ and continuing to react for 2h, thus finishing the reaction. The reaction mixture was sampled and examined for N, N-dimethyltrifluoromethanesulfonamide, and the yield was 97.3% based on trifluoromethanesulfonyl fluoride.
And filtering the reaction solution, distilling at normal pressure to obtain a mixed fraction, and detecting the contents of dimethylamine and isopropanol in the fraction to obtain the recovery rates of the dimethylamine and the isopropanol of 93.4 percent and 95.1 percent. And carrying out negative pressure rectification on the residual reaction liquid to obtain an N, N-dimethyl trifluoromethyl sulfonamide product with the purity of 99.5 percent.
Example three: the reaction was carried out in a 2L four-port glass jacketed kettle equipped with a coolant jacket, a stirrer, a thermometer, and a condenser, the coolant temperature was maintained at-15 ℃, 1218g of ethanol was added to the kettle, and 135g of dimethylamine was introduced to obtain a dimethylamine-ethanol solution. 252g of trifluoromethanesulfonyl chloride liquid was added with stirring and the reaction was maintained at-15 ℃ for 3 hours. And then 102g of sodium ethoxide is added, the mixture is stirred and reacts for 1.5h at the temperature of minus 15 ℃, the temperature is increased to 0 ℃, the reaction is continued for 2h, and the reaction is finished. The reaction mixture was sampled and examined for N, N-dimethyltrifluoromethylsulfonamide at a yield of 98.1% based on trifluoromethylsulfonyl chloride.
And filtering the reaction solution, distilling at normal pressure to obtain mixed fractions, and detecting the contents of dimethylamine and ethanol in the fractions to obtain the dimethylamine and ethanol with recovery rates of 95.3 percent and 93.1 percent. And carrying out negative pressure rectification on the residual reaction liquid to obtain an N, N-dimethyl trifluoromethyl sulfonamide product with the purity of 99.7 percent.
Example four: the reaction was carried out in a 2L four-port glass jacketed kettle equipped with a coolant jacket, a stirrer, a thermometer, and a condenser, with the coolant temperature maintained at-15 deg.C, 1014g of methanol was added to the kettle, and 169g of dimethylamine was passed through to obtain a dimethylamine methanol solution. 252g of trifluoromethanesulfonyl chloride liquid was added with stirring and the reaction was maintained at-15 ℃ for 3.5 hours. Then 81g of sodium methoxide is added, the mixture is stirred and reacted for 1.5h at the temperature of minus 15 ℃, the temperature is increased to 0 ℃, the reaction is continued for 2h, and the reaction is finished. The reaction mixture was sampled and examined for N, N-dimethyltrifluoromethylsulfonamide at a yield of 98.7% based on trifluoromethylsulfonyl chloride.
And filtering the reaction liquid, and then carrying out atmospheric distillation to obtain a mixed fraction, and detecting the contents of dimethylamine and methanol in the fraction to obtain the dimethylamine and ethanol with recovery rates of 92% and 94.4%. And carrying out negative pressure rectification on the residual reaction liquid to obtain an N, N-dimethyl trifluoromethyl sulfonamide product with the purity of 99.6 percent.
Example five: the reaction was carried out in a 2L four-port glass jacketed kettle equipped with a coolant jacket, a stirrer, a thermometer, and a condenser, with the coolant temperature maintained at-25 deg.C, 1014g of methanol was added to the kettle, and 169g of dimethylamine was passed through to obtain a dimethylamine methanol solution. While stirring, 228g of trifluoromethanesulfonyl fluoride gas was introduced thereinto and the reaction was maintained at-25 ℃ for 3.5 hours. Then 105g of potassium methoxide is added, the mixture is stirred and reacts for 1.5 hours at the temperature of minus 30 ℃, the temperature is increased to 0 ℃, the reaction is continued for 2 hours, and the reaction is finished. The reaction mixture was sampled and examined for N, N-dimethyltrifluoromethanesulfonamide, and the yield was 98.6% based on trifluoromethanesulfonyl fluoride.
And filtering the reaction solution, distilling at normal pressure to obtain a mixed fraction, and detecting the contents of dimethylamine and methanol in the fraction to obtain the dimethylamine and methanol with recovery rates of 94.3 percent and 93.1 percent. And carrying out negative pressure rectification on the residual reaction liquid to obtain an N, N-dimethyl trifluoromethyl sulfonamide product with the purity of 99.8 percent.
Example six: the reaction was carried out in a 2L four-port glass-jacketed kettle equipped with a refrigerant jacket, a stirrer, a thermometer, and a condenser, and the mixed fraction containing dimethylamine and ethanol obtained in example 1 was quantitatively added to the reaction kettle (containing 64g of dimethylamine and 1010g of ethanol) while maintaining the temperature of the refrigerant at-30 ℃ and 71g of dimethylamine was added. While stirring, 228g of trifluoromethanesulfonyl fluoride gas was introduced thereinto and the reaction was maintained at-30 ℃ for 3 hours. And then 102g of sodium ethoxide is added, the mixture is stirred at the temperature of minus 30 ℃ to react for 1 hour, and then the temperature is increased to 0 ℃ to continue the reaction for 2 hours, thus finishing the reaction. The reaction mixture was sampled and examined for N, N-dimethyltrifluoromethanesulfonamide, and the yield was 98.0% based on trifluoromethanesulfonyl fluoride.
And filtering the reaction solution, distilling at normal pressure to obtain a mixed fraction, and detecting the contents of dimethylamine and ethanol in the fraction to obtain dimethylamine and ethanol with recovery rates of 94.6 percent and 92.8 percent. And carrying out negative pressure rectification on the residual reaction liquid to obtain an N, N-dimethyl trifluoromethyl sulfonamide product with the purity of 99.7 percent.
Example seven: the reaction was carried out in a 2L four-port glass jacketed kettle equipped with a coolant jacket, a stirrer, a thermometer, and a condenser, the coolant temperature was maintained at-30 deg.C, 541g of methanol was added to the kettle, and 135g of dimethylamine was introduced to obtain dimethylamine-methanol solution. While stirring, 228g of trifluoromethanesulfonyl fluoride gas was introduced thereinto and the reaction was maintained at-30 ℃ for 3.5 hours. Then 153g of calcium methoxide is added, the mixture is stirred and reacted for 1.5h at the temperature of minus 30 ℃, the temperature is increased to 0 ℃, the reaction is continued for 2h, and the reaction is finished. The reaction mixture was sampled and examined for N, N-dimethyltrifluoromethanesulfonamide, and the yield was 98.1% based on trifluoromethanesulfonyl fluoride.
And filtering the reaction solution, distilling at normal pressure to obtain a mixed fraction, and detecting the contents of dimethylamine and methanol in the fraction to obtain the dimethylamine and methanol with recovery rates of 95.3 percent and 94.7 percent. And carrying out negative pressure rectification on the residual reaction liquid to obtain an N, N-dimethyl trifluoromethyl sulfonamide product with the purity of 99.6 percent.
Example eight: the reaction was carried out in a 2L four-port glass jacketed kettle equipped with a coolant jacket, a stirrer, a thermometer, and a condenser, with the coolant temperature maintained at-15 deg.C, 1014g of ethanol was added to the kettle, and 148g of dimethylamine was passed through to obtain a dimethylamine ethanol solution. 252g of trifluoromethanesulfonyl chloride liquid was added with stirring and the reaction was maintained at-15 ℃ for 3 hours. And then 102g of sodium ethoxide is added, the mixture is stirred and reacts for 1.5h at the temperature of minus 15 ℃, the temperature is increased to 0 ℃, the reaction is continued for 2h, and the reaction is finished. The reaction mixture was sampled and examined for N, N-dimethyltrifluoromethylsulfonamide at a yield of 98.3% based on trifluoromethylsulfonyl chloride.
And filtering the reaction solution, distilling at normal pressure to obtain a mixed fraction, and detecting the contents of dimethylamine and ethanol in the fraction to obtain dimethylamine and ethanol with recovery rates of 94.7 percent and 94.2 percent. And carrying out negative pressure rectification on the residual reaction liquid to obtain an N, N-dimethyl trifluoromethyl sulfonamide product with the purity of 99.70 percent.
Comparative example 1: the reaction was carried out in a 2L four-port glass jacketed kettle equipped with a coolant jacket, a stirrer, a thermometer, and a condenser, with the coolant temperature maintained at-30 deg.C, 1014g of ethanol was added to the kettle, and 135g of dimethylamine was passed through to obtain dimethylamine-ethanol solution. 228g of trifluoromethanesulfonyl fluoride gas was introduced while stirring, and the reaction was maintained at-30 ℃ for 3 hours. Heating to 0 ℃ and continuing the reaction for 3h to finish the reaction. The reaction mixture was sampled and examined for N, N-dimethyltrifluoromethanesulfonamide, and the yield was 98.4% based on trifluoromethanesulfonyl fluoride.
And filtering the reaction liquid, then carrying out normal pressure distillation to obtain fractions mainly comprising ethanol and a small amount of dimethylamine, and carrying out negative pressure rectification on the residual reaction liquid to obtain an N, N-dimethyl trifluoromethyl sulfonamide product with the purity of 98.4%, wherein most dimethylamine hydrogen fluoride is remained in the kettle.
Comparative example 2: the reaction was carried out in a 2L four port glass jacketed kettle equipped with a coolant jacket, a stirrer, a thermometer, and a condenser, with the coolant temperature maintained at-15 ℃, 1014g of methanol was added to the kettle, and 135g of dimethylamine was passed through to obtain a dimethylamine methanol solution. 228g of trifluoromethanesulfonyl chloride was added with stirring and the reaction was maintained at-15 ℃ for 3.5 hours. Heating to 0 ℃ and continuing the reaction for 3h to finish the reaction. The reaction mixture was sampled and examined for N, N-dimethyltrifluoromethylsulfonamide at a yield of 98.3% based on trifluoromethylsulfonyl chloride.
And filtering the reaction solution, then distilling at normal pressure to obtain fractions mainly comprising methanol and a small amount of dimethylamine, and carrying out negative pressure rectification on the residual reaction solution to obtain an N, N-dimethyl trifluoromethyl sulfonamide product with the purity of 98.3%, wherein most dimethylamine hydrogen chloride is remained in the kettle.
In examples 1 to 8 and comparative examples 1 to 2, the yield of the solid product was calculated based on the amount of the trifluoromethanesulfonyl halide charged; the purity of the product adopts gas chromatography; the data of the statistical yield, purity and by-product condition are shown in the following table.
Experiment number The synthesis yield is% The rectification purity% Recovery rate of dimethylamine% Recovery rate of alcohol solvent% By-product of the reaction
Example 1 98.20 99.60 95.3 93.3 Sodium fluoride
Example 2 97.30 99.50 93.4 95.1 Sodium fluoride
Example 3 98.00 99.70 95.3 93.1 Sodium chloride
Example 4 98.70 99.60 92.6 94.4 Sodium chloride
Example 5 98.60 99.80 94.3 93.1 Potassium fluoride
Example 6 98.00 99.70 94.6 92.8 Sodium fluoride
Example 7 98.10 99.60 95.3 94.7 Calcium fluoride
Example 8 98.30 99.70 94.7 94.2 Sodium chloride
Comparative example 1 98.40 95.50 0 93.0 Dimethylamine hydrogen fluoride
Comparative example 2 98.30 94.40 0 92.4 Dimethylamine hydrochloride
From the above examples 1 to 8, it was found that the selection of the reaction charge ratio, solvent and alkoxide within the range defined in the present invention did not significantly affect the quality and yield of the product, and the recovery rates of dimethylamine and alcohol solvents of examples 1 to 8 were kept at high levels.
Examples 1-8 compared to comparative example 1,2 give: 1. the reaction synthesis yield is kept high. The reaction solution was directly rectified, and the by-product dimethylamine hydrogen halide in 1,2 in the comparative example was present in the reaction solution, and the dimethylamine hydrogen halide was decomposed by the direct rectification, so that the purity of the product was lower than that in examples 1 to 8. 2. In examples 1 to 8, after the alkoxide was added, dimethylamine and the alcohol solvent were dissociated, and the dimethylamine and the alcohol solvent were separated from the product by atmospheric distillation, so that the method has a significant advantage in the dimethylamine recycling efficiency compared to the comparative example. And the byproducts of the embodiments 1 to 8 are inorganic halogen salts, such as sodium chloride, sodium fluoride and calcium fluoride, which are directly separated from the system, thereby greatly facilitating the post-treatment. Based on these two points, the purity of the products of examples 1 to 8 was 99.5% or more.
In conclusion, the preparation method of the N, N-dimethyl trifluoromethyl sulfonamide provided by the invention not only solves the problems of decomposition and recovery of byproduct dimethylamine hydrogen halide and recovery of alcohol solvent by the technical scheme of firstly constructing an alcohol reaction system and later adding alkoxide, but also obviously reduces the production cost, effectively improves the product purity, is easy to control the reaction, is extremely suitable for industrial production, has high industrial utilization value, and effectively improves the competitive capacity of enterprises.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.

Claims (8)

1. A preparation method of N, N-dimethyl trifluoromethyl sulfonamide comprises the following steps:
1. dissolving dimethylamine in an alcohol solvent at the temperature of-15 to-30 ℃ to form dimethylamine alcohol solution, keeping the low temperature, and adding trifluoromethyl sulfonyl halide into the dimethylamine alcohol solution for reaction; adding alkoxide corresponding to the alcohol solvent after the reaction is completed, and filtering and separating after the reaction is finished to obtain filtrate and solid; the reaction equation is as follows:
CF 3 SO 2 X+(CH 3 ) 2 NH
Figure 956062DEST_PATH_IMAGE001
CF 3 SO 2 N(CH 3 ) 2 + (CH 3 ) 2 NH·HX；
(CH 3 ) 2 NH·HX+M + RO -
Figure 772709DEST_PATH_IMAGE002
(CH 3 ) 2 NH+ ROH+M + X - ↓；
wherein X is selected from one of Cl and F, and M is selected from one of K, na and Ca;
2. distilling the filtrate at normal pressure to separate dimethylamine and alcohol solvent; then rectifying and separating to obtain the N, N-dimethyl trifluoromethyl sulfamide.
2. The process according to claim 1 for the preparation of N, N-dimethyltrifluoromethylsulfonamide, wherein: the alcohol solvent in the first step is selected from one of methanol, ethanol, propanol and isopropanol.
3. The process for preparing N, N-dimethyltrifluoromethylsulfonamide according to claim 2, wherein: in the first step, the alkoxide is selected from methoxide or ethoxide or propoxide or isopropoxide corresponding to the selected alcoholic solvent.
4. The process according to claim 3 for the preparation of N, N-dimethyltrifluoromethylsulfonamide, wherein: the methoxide adopts sodium methoxide, the ethoxide adopts sodium ethoxide, the propoxide adopts sodium propoxide, and the isopropoxide adopts sodium isopropoxide.
5. The process for the preparation of N, N-dimethyltrifluoromethylsulfonamide according to claim 1,2, 3 or 4, wherein: in the first step, the molar ratio of the trifluoromethyl sulfonyl halide, the dimethylamine and the alkoxide is 1:2:1 to 1:2.5:1.
6. the process for the preparation of N, N-dimethyltrifluoromethylsulfonamide according to claim 1,2, 3 or 4, wherein: the dimethylamine separated in the second step and the alcohol solvent are reused for the first step reaction in the preparation process.
7. The process for the preparation of N, N-dimethyltrifluoromethylsulfonamide according to claim 1,2, 3 or 4, wherein: the mass fraction of the dimethylamine alcoholic solution formed in the first step is 10-20%.
8. The process for the preparation of N, N-dimethyltrifluoromethylsulfonamide according to claim 1,2, 3 or 4, wherein: in the first step, after alkoxide is added, the reaction is carried out at the low temperature of-15 to-30 ℃, and then the temperature is increased to 0 ℃ for reaction till the end.
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