Process for the preparation of n-(fluorosulfonyl)dimethylamine

Abstract

This disclosure relates to a method for preparing N-(fluorosulfonyl)dimethylamine, the method comprising the following steps: (1) adding SO2Cl2 and Me2NH to a reactor, and reacting fully to obtain an intermediate product ClSO2NMe2; (2) adding a fluorine source to the intermediate product ClSO2NMe2 obtained in step (1), and reacting fully to obtain a reaction product containing N-(fluorosulfonyl)dimethylamine; and (3) separating N-(fluorosulfonyl)dimethylamine from the reaction product obtained in step (2). This method improves production efficiency and product yield, effectively controls the reaction process, and reduces reaction costs.

Description

Technical Field

[0001] This disclosure relates to the field of electrolytes for secondary batteries, specifically to a method for preparing N-(fluorosulfonyl)dimethylamine. Background Technology

[0002] N-(fluorosulfonyl)dimethylamine (FSO2NMe2) is a viscous, water-immiscible polar liquid with low viscosity and a liquid range of -16.7°C to +149°C. At 25°C, 100 mL of FSO2NMe2 is saturated with 0.475 g of water, and the water content is reduced to approximately 50 ppm by fractional distillation at atmospheric pressure. Pure FSO2NMe2 dissolves many uncharged aprotic substrates and is inert to them. FSO2NMe2 has a flash point higher than its boiling point; placing a Bunsen burner over a boiling beaker of FSO2NMe2 will not ignite its vapor. FSO2NMe2 has been proposed as a solvent or additive for lithium-ion batteries. Currently, FSO2NMe2 is not commercially available in large quantities.

[0003] In the 1930s, FSO2NMe2 was first prepared by a substitution reaction between N-(chlorosulfonyl)dimethylamine (C1SO2NMe2) and potassium, sodium, or zinc fluorides in water (French Patent No. FR806383; German Patent No. DE667544; US Patent No. 2,130,038). FSO2NMe2 was also prepared by reacting C1SO2NMe2 with antimony trifluoride (SbF3) in the presence of antimony pentafluoride (SbF5) (Heap, R., Saunders, BC, Journal of the Chemical Society (Resumed), 1948, 1313-1316), and by reacting ClSO2NMe2 with anhydrous HF at 80-90°C (German Patent No. DE1943233 (1971)). FSO2NMe2 can also be prepared by reacting N,N-dimethylaminosulfonamide (Me2NSO2NH2) with fluorosulfonyl isocyanate (FSO2N=C=O) at 80 °C (Appel, R., Montenarh, M., Chemische Berichte, 1977, 110, 2368-2373). As described below, there are four known examples of the reaction of sulfuryl fluoride (SO2F2) with secondary amines. These four known reactions used a refrigerant (or catalyst). The first reaction of SO2F2 with a secondary amine was carried out in 1948 (Emeleus, HJ, Wood, JF, Journal of the Chemical Society (Resumed), 1948, 2183-2188). In this paper, diethylamine (Et2NH) was added dropwise to a cooled (-78 °C) ether solution of SO2F2 to give the product FSO2NEt2 in a yield of 35%. In 1982, a reaction of SO2F2 with piperidine (HN(CH2)5) was carried out (Padma, DK, Subrahmanya Bhat, V., Vasudeva Murthy, AR, Journal of Fluorine Chemistry, 1982, 20, 425-437). SO2F2 was added to piperidine in an ether at liquid nitrogen temperature, followed by heating. Depending on the amount of piperidine used, FSO2N(CH2)5 or SO2(N(CH2)5)2 was obtained. The patent application of Dong and Sharpless (International Patent Application No. WO2015 / 188120) describes the reaction of two other secondary amines with SO2F2 under ambient conditions. In this application, diallylamine and dialysylamine react with SO2F2 in a solvent in the presence of equimolar amounts of an activator. Specifically, the solvent is described as tetrahydrofuran (THF) and dichloromethane, etc. (page 58, line 15).Dong and Sharpless claim that “activated amines can even react in a buffer solution at pH 8” (page 95, line 14), but they do not provide any examples of activated amines or elaborate further.

[0004] Furthermore, CN109563031A provides a synthetic method in which dimethylamine (Me2NH) reacts with sulfuryl fluoride (SO2F2) to form at least a first phase, the first phase comprising N-(fluorosulfonyl)dimethylamine (FSO2NMe2), tetramethylsulfonamide (SO2(NMe2)2), or a combination thereof. This reaction can also form a second phase, which may contain dimethylamine hydrofluoride (Me2NH2F), and can be separated from the first phase. FSO2NMe2 and SO2(NMe2)2 are then separated from the first phase. However, due to limitations in the reactants and starting materials, the reactants cannot be efficiently converted to FSO2NMe2, resulting in low conversion efficiency. In the conventional reaction of sulfuryl fluoride (SO₂F₂), the reaction formula is generally SO₂F₂ + 2Me₂NH = FSO₂NMe₂ + Me₂NH₂F. Even under ideal conditions, this reaction generates other products, such as Me₂NH₂F. Therefore, the utilization efficiency of sulfuryl fluoride and Me₂NH in a single reaction is only about 50% under complete reaction conditions. Otherwise, the other product Me₂NH₂F needs to be recovered and reused, increasing the complexity of the reaction and reducing its efficiency. Furthermore, this is a one-step reaction with relatively harsh reaction conditions and weak control over the reaction process, which can lead to a decrease in purity and yield.

[0005] Therefore, there is a need in this field to develop a more efficient and low-cost preparation method for the synthesis of FSO2NMe2. Summary of the Invention

[0006] The purpose of this disclosure is to provide a novel method for preparing N-(fluorosulfonyl)dimethylamine, which employs a two-step process, improving production efficiency and product yield, effectively controlling the reaction process, and reducing reaction costs.

[0007] This disclosure provides a method for preparing N-(fluorosulfonyl)dimethylamine, the method comprising the following steps:

[0008] (1) SO2Cl2 and Me2NH were added to the reactor and reacted completely to obtain the intermediate product ClSO2NMe2;

[0009] (2) A fluorine source is added to the intermediate product ClSO2NMe2 obtained in step (1), and after sufficient reaction, a reaction product containing N-(fluorosulfonyl)dimethylamine is obtained; and

[0010] (3) N-(fluorosulfonyl)dimethylamine was isolated from the reaction product obtained in step (2).

[0011] In a preferred embodiment, in steps (1) and / or (2), the reaction is carried out in a solvent and / or water, said solvent being an aprotic polar solvent.

[0012] In another preferred embodiment, the aprotic polar solvent is selected from the group consisting of dichloromethane, diethyl ether, tetrahydrofuran, 2-methyltetrahydrofuran, methylcyclopentyl ether, methyl tert-butyl ether, acetonitrile, propionitrile, butyronitrile, toluene, and any combination thereof.

[0013] In another preferred embodiment, in steps (1) and / or (2), the reaction is carried out in an organic solvent, which is a nonpolar or weakly polar organic solvent.

[0014] In another preferred embodiment, the organic solvent is selected from the group consisting of methanol, ethanol, dichloromethane, diethyl ether, tetrahydrofuran, 2-methyltetrahydrofuran, methylcyclopentyl ether, methyl tert-butyl ether, acetonitrile, propionitrile, butyronitrile, toluene, and any combination thereof.

[0015] In another preferred embodiment, in steps (1) and / or (2), an organic base and / or an inorganic base are added to the reaction, preferably the organic base is added slowly to the reactor.

[0016] In another preferred embodiment, the organic base is at least one of trimethylamine, triethylamine, tri-n-propylamine, tri-n-butylamine, pyridine, piperidine, and piperazine; and the inorganic base is at least one of KOH, LiOH, NaOH, Na2CO3, NaHCO3, Ca(OH)2, Mg(OH)2, and K2CO3.

[0017] In another preferred embodiment, in step (1) and / or (2), a catalyst is added to the reaction, said catalyst comprising bismuth trifluoride.

[0018] In another preferred embodiment, in step (1), the molar ratio of SO2Cl2 to Me2NH is 0.2:1 to 4:1, preferably 1:1.9 to 1:2.5.

[0019] In another preferred embodiment, in step (1), when an organic base is added, the molar ratio of SO2Cl2 to Me2NH is 0.5:1 to 2:1, preferably 0.8:1 to 1:1.2.

[0020] In another preferred embodiment, in step (2), the fluorine source includes potassium fluoride, ammonium fluoride, hydrogen fluoride and hydrogen fluoride complex, and the molar ratio of Me2NH to the fluorine source is 0.5:1 to 2:1, preferably 0.8:1 to 1:1.2.

[0021] In another preferred embodiment, the method further includes: extracting and / or purifying the intermediate product ClSO2NMe2 obtained in step (1) before performing step (2).

[0022] In another preferred embodiment, in step (3), the reaction product obtained in step (2) is treated by filtration, concentration, washing and / or distillation to separate N-(fluorosulfonyl)dimethylamine, preferably by vacuum distillation of the reaction solution to separate N-(fluorosulfonyl)dimethylamine.

[0023] In another preferred embodiment, in step (1), the reaction temperature of Me2NH and SO2Cl2 is -30°C to 120°C, preferably -20°C to 60°C, and the reaction pressure is 20-40 kPa.

[0024] In another preferred embodiment, in step (1), the reactor is a batch reactor or a continuous flow reactor; preferably, the reaction is carried out in an open reactor or a sealed reactor, more preferably, the reaction is carried out in a sealed reactor.

[0025] Beneficial effects:

[0026] The method described in this application enables the efficient large-scale production of FSO2NMe2 at very low cost. The precursors SO2Cl2 and Me2NH are both inexpensive and available in tonnes. When water is used as a solvent, the product FSO2NMe2 is simply removed from the aqueous layer and distilled. Using the method described in this application, very large quantities of FSO2NMe2 can be produced in a short time with minimal labor. Detailed Implementation

[0027] The "range" disclosed herein is defined by a lower limit and an upper limit. A given range is defined by selecting a lower limit and an upper limit, which define the boundaries of a particular range. Ranges defined in this way can include or exclude endpoints and can be arbitrarily combined; that is, any lower limit can be combined with any upper limit to form a range. For example, if ranges of 60-120 and 80-110 are listed for a specific parameter, it is expected that ranges of 60-110 and 80-120 are also expected. Furthermore, if minimum range values ​​of 1 and 2 are listed, and if maximum range values ​​of 3, 4, and 5 are listed, then the following ranges are all expected: 1-3, 1-4, 1-5, 2-3, 2-4, and 2-5. In this application, unless otherwise stated, the numerical range "ab" represents a shortened representation of any combination of real numbers between a and b, where a and b are real numbers. For example, the numerical range "0-5" indicates that all real numbers between "0-5" have been listed in this article; "0-5" is simply a shortened representation of these numerical combinations. Furthermore, when a parameter is stated as an integer ≥2, it is equivalent to disclosing that the parameter is, for example, an integer such as 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc.

[0028] Unless otherwise specified, all embodiments and preferred embodiments mentioned herein can be combined to form new technical solutions. Similarly, unless otherwise specified, all technical features and preferred features mentioned herein can be combined to form new technical solutions.

[0029] In this application, unless otherwise specified, the terms "comprising" and "including" as used herein are open-ended or closed-ended. For example, "comprising" and "including" may mean that other components not listed may also be included, or that only the listed components may be included.

[0030] In this description, unless otherwise stated, the term "or" is inclusive. For example, the phrase "A or B" means "A, B, or both A and B". More specifically, the condition "A or B" is satisfied by any of the following conditions: A is true (or exists) and B is false (or does not exist); A is false (or does not exist) and B is true (or exists); or both A and B are true (or exist).

[0031] It should be understood that in the description of this disclosure, the terms "first," "second," etc., are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Therefore, a feature defined with "first," "second," etc., may explicitly or implicitly include one or more of that feature. In the description of this disclosure, unless otherwise stated, "a plurality of" means two or more.

[0032] To address the shortcomings of existing methods for preparing N-(fluorosulfonyl)dimethylamine, which use a one-step reaction, resulting in relatively harsh reaction conditions, weak control over the reaction process, and decreased purity and yield, this application employs a two-step method for the synthesis of N-(fluorosulfonyl)dimethylamine. This method allows for better control of reaction conditions, thereby improving product selectivity, reducing side reactions, and enabling better purification, thus overcoming the deficiencies of existing technologies.

[0033] This disclosure provides a method for preparing N-(fluorosulfonyl)dimethylamine, the method comprising the following steps:

[0034] (1) SO2Cl2 and Me2NH were added to the reactor and reacted completely to obtain the intermediate product ClSO2NMe2;

[0035] (2) A fluorine source is added to the intermediate product ClSO2NMe2 obtained in step (1), and after sufficient reaction, a reaction product containing N-(fluorosulfonyl)dimethylamine is obtained; and

[0036] (3) N-(fluorosulfonyl)dimethylamine was isolated from the reaction product obtained in step (2).

[0037] Preferably, in steps (1) and / or (2), an organic base and / or an inorganic base are added to the reaction; more preferably, the organic base is slowly added to the reactor.

[0038] Preferably, the organic base is at least one of trimethylamine, triethylamine, tri-n-propylamine, tri-n-butylamine, pyridine, piperidine, and piperazine; and the inorganic base is at least one of KOH, LiOH, NaOH, Na2CO3, NaHCO3, Ca(OH)2, Mg(OH)2, and K2CO3.

[0039] In this disclosure, without the addition of an organic base, the molar ratio of SO2Cl2 to Me2NH is preferably 0.2:1 to 4:1, more preferably 1:1.9 to 1:2.5. The reaction formula for the first step is generally SO2Cl2 + 2Me2NH = ClSO2NMe2 + Me2NH2Cl; taking anhydrous potassium fluoride as an example, the reaction formula for the second step is ClSO2NMe2 + KF = FSO2NMe2 + KCl. During the reaction, the utilization rate of F atoms in the reactants can be more effectively improved, increasing its theoretical utilization rate to 100%. However, the utilization rate of Me2NH is still only half of its own.

[0040] In this disclosure, when an organic base is added, the molar ratio of SO2Cl2 to Me2NH is preferably 0.5:1 to 2:1, more preferably 0.8:1 to 1:1.2. Taking triethylamine as an example, the reaction formula for the first step is generally SO2Cl2 + Me2NH + Et3N = ClSO2NMe2 + Et3N.HCl; taking anhydrous potassium fluoride as an example, the reaction formula for the second step is ClSO2NMe2 + KF = FSO2NMe2 + KCl. During the reaction, the utilization rate of F atoms in the reactants can be improved more effectively, increasing its theoretical utilization rate to 100%, and the utilization rate of Me2NH can also reach an effective 100%. After the organic base is added, triethylamine chloride (Et3N.HCl) is generated, thereby preventing interference from other products on the reaction system.

[0041] Preferably, in steps (1) and / or (2), the reaction is carried out in a solvent and / or water.

[0042] Preferably, the solvent is an organic solvent, which is a non-polar organic solvent or a weakly polar organic solvent.

[0043] Preferably, the organic solvent is selected from the group consisting of methanol, ethanol, dichloromethane, diethyl ether, tetrahydrofuran, 2-methyltetrahydrofuran, methylcyclopentyl ether, methyl tert-butyl ether, acetonitrile, propionitrile, butyronitrile, toluene, and any combination thereof.

[0044] Preferably, the solvent is a low-boiling-point aprotic polar solvent.

[0045] Preferably, the aprotic polar solvent includes, but is not limited to: dichloromethane, diethyl ether, tetrahydrofuran, 2-methyltetrahydrofuran, methylcyclopentyl ether, methyl tert-butyl ether, acetonitrile, propionitrile, butyronitrile, toluene, and any combination thereof. Among these, in acetonitrile, FSO2NMe2 exhibits strong reactivity with Me2NH at ambient temperature. Therefore, in this disclosure, solvents other than water are used, and the temperature should be sufficiently low (down to the liquidus point of the solvent system) to minimize the formation of byproducts.

[0046] In this disclosure, the reaction in anhydrous solvent can be carried out completely at pressures below atmospheric pressure.

[0047] In this disclosure, anhydrous solvents can combine with water to produce aqueous solvents.

[0048] In this disclosure, an anhydrous solvent that is immiscible with water can combine with water to produce a two-phase solvent system.

[0049] In this disclosure, when the invention is carried out under aqueous and non-aqueous conditions, the molar ratio of dimethylamine to thiocyanate chloride is a parameter that needs to be controlled.

[0050] In this disclosure, the molar ratio (Me2NH / SO2Cl2) that can be used is about 0.2:1 to about 4:1.

[0051] In this disclosure, the molar ratio is adjusted to form sufficient FSO2NMe2 to dissolve all by-reaction products in the lower layer, thereby enabling the process stream to be separated into two liquids, which can then be distilled off from the lower layer.

[0052] In this disclosure, tertiary amines (such as triethylamine) can be added to the reaction vessel or used simply as a solvent, and the molar ratio of Me2NH:SO2ClF can be reduced.

[0053] In this disclosure, 100% Me2NH may also be used as a solvent, or an anhydrous solvent may be used, or water may be used as part or all of the solvent.

[0054] In this disclosure, an excess of liquid Me2NH can be used as a solvent for the reaction.

[0055] In this disclosure, water can be used as the solvent, the reaction is carried out in water, and the lower layer of FSO2NMe2 can be separated and distilled without any washing. Furthermore, the byproducts are only in the lower layer and are easily separated from FSO2NMe2 by vacuum distillation.

[0056] Preferably, in step (1) and / or (2), a catalyst is added to the reaction, said catalyst including bismuth trifluoride, etc.

[0057] In this disclosure, in step (2), the fluorine source includes potassium fluoride, ammonium fluoride, hydrogen fluoride, and hydrogen fluoride complexes, etc.

[0058] In this disclosure, the molar ratio of Me2NH to the fluorine source is preferably 0.5:1 to 2:1, more preferably 0.8:1 to 1:1.2.

[0059] Preferably, the method further includes: before performing step (2), extracting and / or purifying the intermediate product ClSO2NMe2 obtained in step (1) to separate the intermediate product ClSO2NMe2 with higher purity before performing the reaction in step (2).

[0060] Preferably, to save reaction time and steps, a solvent or catalyst can be added to the reaction in step (2), so that the intermediate reaction product obtained in step (1) is not processed and the reaction in step (2) is carried out directly.

[0061] In this disclosure, in step (3), the reaction product obtained in step (2) is treated by means of filtration, concentration, washing and / or distillation to separate N-(fluorosulfonyl)dimethylamine, preferably by vacuum distillation of the reaction solution to separate N-(fluorosulfonyl)dimethylamine.

[0062] Preferably, in step (1), the reaction temperature of Me2NH and SO2Cl2 is about -30°C to 120°C, more preferably -20°C to about 60°C, and the reaction pressure is about 20-40 kPa.

[0063] In this disclosure, in step (1), the reactor is a batch reactor or a continuous flow reactor.

[0064] Preferably, the reaction is carried out in an open or sealed reactor, and more preferably, the reaction is carried out in a sealed reactor.

[0065] In the following, the preparation of N-(fluorosulfonyl)dimethylamine using the method of the present invention is characterized based on specific embodiments. However, it should be specifically noted that the scope of protection of this application is defined by the claims, and not limited to the specific embodiments.

[0066] Example

[0067] Unless otherwise stated, all raw materials used in this application are analytical grade, and all water is deionized water.

[0068] General procedure: Add dimethylamine to the high-pressure reactor, cool, and evacuate to a constant static pressure; introduce thioyl chloride into the top space under maximum stirring, add or not add an organic base, and cool to maintain the temperature to obtain the intermediate product ClSO2NMe2; vent the high-pressure reactor, add a fluorine source (such as anhydrous potassium fluoride), add or not add an organic base, open and separate the contents with a funnel, and distill the lower layer material under reduced pressure to obtain pure FSO2NMe2.

[0069] Examples 1-6: SO2Cl2 reacts with anhydrous Me2NH without acid-binding agent.

[0070] The reaction equation for the first step is SO₂Cl₂ + 2Me₂NH = ClSO₂NMe₂ + Me₂NH₂Cl; using anhydrous potassium fluoride, the reaction equation for the second step is ClSO₂NMe₂ + KF = FSO₂NMe₂ + KCl. The ratio of SO₂Cl₂ / Me₂NH ranges from 0.2:1 to 4:1; the ratio of Me₂NH / anhydrous potassium fluoride ranges from 0.5:1 to 2:1.

[0071] Dimethylamine was added to a high-pressure reactor, cooled to 30°C, and evacuated to a constant static pressure of 20 kPa. Thionyl chloride was introduced into the top space under maximum stirring, and the reaction was carried out for 30 minutes. The reactor was then cooled to maintain the temperature at 30°C to obtain the intermediate product ClSO2NMe2. The high-pressure reactor was vented, anhydrous potassium fluoride was added, and the reaction was carried out for 30 minutes. The reactor was then opened and the contents were separated using a funnel. The lower layer of material was subjected to vacuum distillation to obtain pure FSO2NMe2.

[0072] The yield of FSO2NMe2 and the dimethylamine utilization were measured. See Table 1 below.

[0073] Comparative Examples 1-6: SO2F2 reacts with Me2NH without acid-binding agent.

[0074] The reaction SO2F2 + 2Me2NH = FSO2NMe2 + Me2NH2F. The ratio of SO2F2 / Me2NH ranges from 0.2:1 to 4:1.

[0075] Dimethylamine was added to the high-pressure reactor, cooled to 30°C, and evacuated to a constant static pressure of 20 kPa. Thionyl fluoride was introduced into the top space under maximum stirring, reacted for 30 minutes, and cooled to maintain the temperature at 30°C. The high-pressure reactor was vented, opened, and the contents were separated by a funnel. The lower layer was distilled under reduced pressure to obtain pure FSO2NMe2.

[0076] The yield of FSO2NMe2 and the dimethylamine utilization were measured. See Table 1 below.

[0077] As can be seen from Table 1, in Examples 1-6, the yield and dimethylamine utilization were both higher compared to the case using SO2F2.

[0078] Examples 7-12: SO2Cl2 reacts with Me2NH, with triethylamine acting as an acid-binding agent.

[0079] The reaction equation for the first step is SO2Cl2 + 2Me2NH = ClSO2NMe2 + Me2NH2Cl; using anhydrous potassium fluoride, the reaction equation for the second step is ClSO2NMe2 + KF = FSO2NMe2 + KCl, the ratio of SO2Cl2 / Me2NH is between 0.5:1 and 2:1; the ratio of Me2NH / anhydrous potassium fluoride is between 0.5:1 and 2:1.

[0080] Dimethylamine and triethylamine (1, 1.1, or 1.2 equivalents (eq)) were added to a high-pressure reactor, cooled to 30°C, and evacuated to a constant static pressure of 20 kPa. Thionyl chloride was introduced into the top space under maximum stirring, and the reaction was carried out for 30 minutes. The reactor was then cooled to maintain the temperature at 30°C to obtain the intermediate product ClSO2NMe2. The high-pressure reactor was then vented, anhydrous potassium fluoride was added, and the reaction was carried out for 30 minutes. The reactor was then opened and the contents were separated using a funnel. The lower layer was subjected to vacuum distillation to obtain pure FSO2NMe2.

[0081] The yield of FSO2NMe2 and the dimethylamine utilization were measured. See Table 2 below.

[0082] Comparative Examples 7-12: SO2F2 reacts with Me2NH, and triethylamine is present as an acid-binding agent.

[0083] The reaction SO2F2 + 2Me2NH = FSO2NMe2 + Me2NH2F has a SO2F2 / Me2NH ratio ranging from 0.5:1 to 2:1.

[0084] Dimethylamine and triethylamine (1, 1.1, or 1.2 eq) were added to the high-pressure reactor, cooled to 30°C, and evacuated to a constant static pressure of 20 kPa. Thionyl fluoride was introduced into the top space under maximum stirring, reacted for 30 minutes, and cooled to maintain the temperature at 30°C. The high-pressure reactor was vented, opened, and the contents were separated using a funnel. The lower layer was subjected to vacuum distillation to obtain pure FSO2NMe2.

[0085] The yield of FSO2NMe2 and the dimethylamine utilization were measured. See Table 2 below.

[0086] As can be seen from Table 2, in the cases of Examples 7-12, the yield and dimethylamine utilization were both higher compared to the case using SO2F2.

[0087] Table 1: Acid-free agents

[0088]

[0089] (1) The result is calculated by dividing the molar amount of FSO2NMe2 obtained by the molar amount of SO2Cl2 or SO2F2 added.

[0090] (2) The result is calculated by dividing the molar amount of dimethylamine in FSO2NMe2 by the molar amount of dimethylamine added.

[0091] Table 2: Triethylamine as an acid-binding agent

[0092]

Claims

1. A method for preparing N-(fluorosulfonyl)dimethylamine, characterized in that, The method includes the following steps: (1) SO2Cl2 and Me2NH were added to the reactor and reacted completely to obtain the intermediate product ClSO2NMe2; (2) A fluorine source is added to the intermediate product ClSO2NMe2 obtained in step (1), and after sufficient reaction, a reaction product containing N-(fluorosulfonyl)dimethylamine is obtained; and (3) N-(fluorosulfonyl)dimethylamine was isolated from the reaction product obtained in step (2).

2. The method as described in claim 1, characterized in that, In steps (1) and / or (2), the reaction is carried out in a solvent and / or water, wherein the solvent is an aprotic polar solvent.

3. The method as described in claim 2, characterized in that, The aprotic polar solvent is selected from the group consisting of: dichloromethane, diethyl ether, tetrahydrofuran, 2-methyltetrahydrofuran, methylcyclopentyl ether, methyl tert-butyl ether, acetonitrile, propionitrile, butyronitrile, toluene, and any combination thereof.

4. The method as described in claim 1, characterized in that, In steps (1) and / or (2), the reaction is carried out in an organic solvent, which is a nonpolar or weakly polar organic solvent.

5. The method as described in claim 4, characterized in that, The organic solvent is selected from the group consisting of methanol, ethanol, dichloromethane, diethyl ether, tetrahydrofuran, 2-methyltetrahydrofuran, methylcyclopentyl ether, methyl tert-butyl ether, acetonitrile, propionitrile, butyronitrile, toluene, and any combination thereof.

6. The method as described in claim 1, characterized in that, In steps (1) and / or (2), an organic base and / or an inorganic base are added to the reaction, preferably the organic base is added slowly to the reactor.

7. The method as described in claim 6, characterized in that, The organic base is at least one of trimethylamine, triethylamine, tri-n-propylamine, tri-n-butylamine, pyridine, piperidine, and piperazine; the inorganic base is at least one of KOH, LiOH, NaOH, Na2CO3, NaHCO3, Ca(OH)2, Mg(OH)2, and K2CO3.

8. The method as described in claim 1, characterized in that, In steps (1) and / or (2), a catalyst is added to the reaction, said catalyst comprising bismuth trifluoride.

9. The method as described in claim 1, characterized in that, In step (1), the molar ratio of SO2Cl2 to Me2NH is 0.2:1 to 4:1, preferably 1:1.9 to 1:2.

5.

10. The method as described in claim 6, characterized in that, In step (1), when an organic base is added, the molar ratio of SO2Cl2 to Me2NH is 0.5:1 to 2:1, preferably 0.8:1 to 1:1.

2.

11. The method as described in claim 1, characterized in that, In step (2), the fluorine source includes potassium fluoride, ammonium fluoride, hydrogen fluoride and hydrogen fluoride complex, and the molar ratio of Me2NH to the fluorine source is 0.5:1 to 2:1, preferably 0.8:1 to 1:1.

2.

12. The method as described in claim 1, characterized in that, The method further includes: extracting and / or purifying the intermediate product ClSO2NMe2 obtained in step (1) before performing step (2).

13. The method as described in claim 1, characterized in that, In step (3), the reaction product obtained in step (2) is treated by filtration, concentration, washing and / or distillation to separate N-(fluorosulfonyl)dimethylamine, preferably by vacuum distillation of the reaction solution to separate N-(fluorosulfonyl)dimethylamine.

14. The method as described in claim 1, characterized in that, In step (1), the reaction temperature of Me2NH and SO2Cl2 is -30℃ to 120℃, preferably -20℃ to 60℃, and the reaction pressure is 20-40kPa.

15. The method as described in claim 1, characterized in that, In step (1), the reactor is a batch reactor or a continuous flow reactor; preferably, the reaction is carried out in an open reactor or a sealed reactor, more preferably, the reaction is carried out in a sealed reactor.

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