CN113862708A - Method for electrochemically synthesizing beta-cyano-bis-phenylsulfonyl imide compound - Google Patents

Method for electrochemically synthesizing beta-cyano-bis-phenylsulfonyl imide compound Download PDF

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CN113862708A
CN113862708A CN202111291076.0A CN202111291076A CN113862708A CN 113862708 A CN113862708 A CN 113862708A CN 202111291076 A CN202111291076 A CN 202111291076A CN 113862708 A CN113862708 A CN 113862708A
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陈依漪
孔宪强
陈小卉
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Changzhou Institute of Technology
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Abstract

The invention discloses a method for electrochemically synthesizing beta-cyanobiphenylsulfimide compounds, which is characterized in that alkene or derivatives thereof, cyanobenzophenone and dibenzenesulfonylimide are used as reaction raw materials, acetonitrile is used as a solvent, tetrabutylammonium acetate is used as an electrolyte, and the compounds are electrochemically synthesized under the protection of inert atmosphere. The method has simple synthesis steps, and solves the problems of narrow range of toxic cyano reagent, metal catalyst and substrate used in the conventional synthesis method; the synthesis of the invention can be carried out at room temperature without adding any initiator, the reaction condition is mild, and the product has no metal residue. Because the electrochemical reaction only needs to be electrified, complex photochemical reaction equipment is not needed, and the requirement on instrument equipment is low; in addition, the electric energy is directly applied to the reaction without energy conversion, thereby avoiding energy waste and saving energy consumption, and the method greatly reduces the reaction cost.

Description

Method for electrochemically synthesizing beta-cyano-bis-phenylsulfonyl imide compound
Technical Field
The invention relates to the technical field of electrochemical synthesis, in particular to a method for electrochemically synthesizing beta-cyano-bis-phenylsulfonylimide compounds.
Background
In the field of organic synthesis, a beta-cyano-bis-phenylsulfonylimide compound is a very common cyano-and-bis-phenylsulfonylimide compound and has wide application in the fields of natural products, medicaments, functional materials and the like. The structure of the beta-cyano-bis-benzene sulfonyl imide compound is shown as the following formula (II), (wherein R represents different functional groups, specifically alkyl, aryl or derivatives thereof). And cyano is an important and common functional group, and in a chemical reaction, cyano can be converted into various functional groups such as carboxylic acid, amide, aldehyde, ketone, amino acid and the like through a series of transformations, so that different compounds can be prepared.
Figure BDA0003334841570000011
At present, beta-cyanobenzenesulfonimide compounds are mainly prepared by alpha, beta-unsaturated ketone through conjugate cyanidation addition reaction, but the cyanide source used at present is a cyanide reagent with high toxicity, such as hydrocyanic acid, trimethylsilylcyano, potassium cyanide and the like. Olefin is a simple and easily-obtained raw material, and the double-functionalization reaction of olefin can quickly construct complex molecules and has wide application in organic synthesis. A group of subjects of the prior professor reported in recent years cyanylation of olefins (references: H.Zhang, W.Pu, T.Xiong, Y.Li, X.ZHou, K.Sun, Q.Liu and Q.Zhang, Copper-catalyst interaction and catalysis of olefins [ J ]. Angew.chem.int.Ed.,2013,52, 2529). The method for preparing the beta-cyanobenzene bissuccinimide compound has the disadvantages of using trimethyl silane with high toxicity, using copper metal for catalysis, having high cost, narrow substrate range, being not environment-friendly and the like, and the reaction process is shown as the following formula (III). Therefore, the development of a method for synthesizing the beta-cyano-bis-phenylsulfonyl imide compound, which has the advantages of mild reaction conditions, simple synthesis steps, low cost and more environmental protection, has important significance.
Figure BDA0003334841570000021
Disclosure of Invention
Aiming at the problems of high toxicity of raw materials, high synthesis cost, narrow substrate range, environment-friendliness in the synthesis process and the like in the conventional beta-cyanobiphenylimide compound synthesis process, the invention provides the electrochemical synthesis method of the beta-cyanobiphenylimide compound, which is green and environment-friendly, simple in synthesis process, mild in reaction conditions and low in synthesis cost.
The invention is realized by the following technical scheme:
the method for electrochemically synthesizing the beta-cyanobiphenylsulfimide compound is characterized in that the beta-cyanobiphenylsulfimide compound takes olefin or derivatives thereof, Cyanobenzophenone (CBX) and dibenzenesulfonimide (BBI) as reaction raw materials, acetonitrile as a solvent, and tetrabutylammonium acetate (n-Bu)4NOAc) is used as electrolyte and is obtained by electrochemical synthesis under the protection of inert atmosphere;
the alkene or the derivative thereof has a structural general formula shown in a formula (I);
Figure BDA0003334841570000022
in the formula R1Represents an alkyl group, an aromatic group or a derivative thereof.
The beta-cyano-bis-phenylsulfonylimide compound is prepared by taking olefin or derivatives thereof, cyano-benzoxazolone and bis-phenylsulfonylimide as raw materials and acetonitrile as a solvent through an electrochemical method, and the preparation method has the advantages of mild reaction conditions, low cost and high product yield.
Specifically, tetrabutylammonium acetate in the present invention functions to promote the formation of N-C bonds by proton-coupling electron transfer of H atoms in the N-H bonds (refer to: X.Hu, G.T.Zhang, L.Nie, T.G.Kong and A.W.Lei, Electrochemical oxidation induced interfacial electron analysis C-H immunization [ J ]. Nat.Commun.,2019,10, 5467).
Further, the method for electrochemically synthesizing the beta-cyanobenzene bissuccinimide compound comprises the following specific steps:
(1) in a nitrogen atmosphere, adding the olefin or the derivative thereof, the cyanobenzophenone and the bis-benzenesulfonylimide into an electrolytic cell filled with the acetonitrile in proportion, and uniformly stirring to obtain a mixture;
(2) putting the electrolyte into the mixture, taking a platinum sheet as an anode and a graphite rod as a cathode, and introducing constant current to carry out electrochemical reaction;
(3) and after the reaction is finished, taking out the reaction liquid, adding water, stirring, extracting, drying and purifying to obtain the beta-cyano-bis-benzene sulfimide compound.
Further, the method for electrochemically synthesizing the beta-cyanobenzene bissuccinimide compound comprises the following steps: in a nitrogen atmosphere, enabling the olefin or the derivative thereof, the cyanobenzophenone and the bisbenzenesulfonimide to react according to a molar ratio of 1: (1-3): (1-5) to an electrolytic cell containing the acetonitrile, and stirring for 10-20 minutes to obtain a mixture.
Further, the method for electrochemically synthesizing the beta-cyanobenzene bissuccinimide compound comprises the following steps: the molar ratio between the alkene or derivative thereof, the cyanobenzophenone and the bisbenzenesulfonylimide is 1: 1: 1.5.
further, the method for electrochemically synthesizing the beta-cyanobenzene bissuccinimide compound comprises the following steps: the molar volume ratio of the olefin or the derivative thereof to the acetonitrile in the step (1) is 0.05-0.1 mol/L. Preferably, the molar volume ratio of the olefin or derivative thereof to the acetonitrile is 0.075 mol/L.
Further, the method for electrochemically synthesizing the beta-cyanobenzene bissuccinimide compound comprises the following steps: and (2) putting the electrolyte into the mixture, taking a platinum sheet as an anode and a graphite rod as a cathode, and introducing a constant current of 5-8mA to perform electrochemical reaction for 6-8 hours.
Further, the method for electrochemically synthesizing the beta-cyanobenzene bissuccinimide compound comprises the following steps: the molar volume ratio of the electrolyte to the mixture in the step (2) is 0.05-0.1 mol/L. Preferably, the molar volume ratio of the catalyst to the mixture is 0.075 mol/L.
Further, the method for electrochemically synthesizing the beta-cyanobenzene bissuccinimide compound comprises the following steps: and (3) after the reaction in the step (3) is finished, taking out the reaction liquid, adding the reaction liquid into a separating funnel, adding water, stirring, extracting the water phase by using ethyl acetate, drying the organic phase by using anhydrous sodium sulfate, and finally performing column chromatography purification and separation to obtain the beta-cyanobenzenesulfonimide compound.
Specifically, the invention provides a method for directly preparing a beta-cyano-bis-benzene sulfonyl imide compound by taking olefin, cyano-benzo oxygen ketone (CBX) and bis-benzene sulfonyl imide (BBI) as raw materials and acetonitrile as a solvent through electrochemistry in a nitrogen atmosphere. The method provided by the invention has simple synthesis steps, and solves the problems of narrow range of toxic cyano reagent, metal catalyst and substrate used in the conventional synthesis method. The synthesis reaction of the invention does not need to add any initiator, and only needs to be carried out at room temperature, the reaction condition is mild, and simultaneously, no metal residue exists in the product. Because the electrochemical reaction only needs to be electrified, complex photochemical reaction equipment is not needed, and the requirement on instrument equipment is low; in addition, the electric energy is directly applied to the reaction without energy conversion, thereby avoiding energy waste and saving energy consumption, and the synthesis method of the invention also greatly reduces the reaction cost.
The invention has the beneficial effects that:
(1) the invention provides an electrochemical synthesis method of a beta-cyano-group bis-benzene sulfimide compound, which is environment-friendly, simple in synthesis steps, mild in reaction conditions and low in cost.
(2) Compared with the existing synthesis method of the beta-cyanobiphenylsulfimide compound, the electrochemical synthesis method of the beta-cyanobiphenylsulfimide compound provided by the invention has low requirements on instruments and equipment, does not use a metal catalyst, saves the cost, has mild reaction conditions, simple operation steps and short reaction time, can be widely applied to the fields of scientific research, medical treatment, industry and the like, and has wide application prospects.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for electrochemically synthesizing beta-cyano-bis-phenylsulfonyl imide compounds comprises the following specific steps:
(1) in a nitrogen atmosphere, 0.3mmol (35.4mg) of 3-methylstyrene, 0.3mmol (81.9mg) of cyanobenzophenone and 0.45mmol (133.65mg) of bisbenzenesulfonylimide were charged into a 10 mL-volume diaphragm-free electrolytic cell, and then 4mL of acetonitrile was further charged into the electrolytic cell and stirred for 10 minutes to dissolve the starting materials to obtain a mixture;
(2) adding electrolyte (n-Bu) to the mixture4NOAc), inserting two electrodes into an electrolytic cell, using a platinum sheet (10 × 10 × 0.2mm) as an anode and a graphite rod (I ═ 6mm) as a cathode, and introducing 5mA of constant current to perform electrochemical reaction for 8 hours; the molar volume ratio of the catalyst to the mixture is 0.075 mol/L;
(3) after the reaction is finished, taking out the reaction liquid, adding the reaction liquid into a separating funnel, adding 20mL of water, stirring, extracting a water phase by using ethyl acetate, drying an organic phase by using anhydrous sodium sulfate, and finally performing column chromatography purification and separation to obtain 89.9mg of a product, namely, the nitrogen- (2-cyano-2- (m-tolyl) ethyl) -nitrogen- (benzenesulfonyl) benzenesulfonamide (beta-cyanobenzenesulfonamide compounds), wherein the yield of the product is calculated to be 64%; the structural formula of the obtained product is shown as follows:
Figure BDA0003334841570000061
1H NMR(600MHz,Chloroform-d)δ8.07–8.00(m,4H),7.74–7.68(m,2H),7.61–7.54(m,4H),7.32(t,J＝7.8Hz,1H),7.25–7.19(m,3H),4.52(dd,J＝9.1,6.3Hz,1H),4.21(dd,J＝15.3,9.1Hz,1H),3.95(dd,J＝15.3,6.3Hz,1H),2.38(s,3H).13C NMR(151MHz,CDCl3)δ139.49,138.44,134.44,132.21,129.86,129.46,129.23,128.85,128.81,125.18,118.83,51.13,21.40.
the method for calculating the yield of the product comprises the following steps: the yield is the amount of the target product (actually) produced per the theoretical amount of the target product × 100%.
Example 2
A method for electrochemically synthesizing beta-cyano-bis-phenylsulfonyl imide compounds comprises the following specific steps:
(1) in a nitrogen atmosphere, 0.3mmol (36.6mg) of 4-fluorostyrene, 0.3mmol (81.9mg) of cyanobenzophenone and 0.45mmol (133.65mg) of bisbenzenesulfonylimide were added to a 10 mL-volume diaphragm-free electrolytic cell, and then 4mL of acetonitrile was added to the electrolytic cell and stirred for 15 minutes to dissolve the starting materials to obtain a mixture;
(2) adding electrolyte (n-Bu) to the mixture4NOAc), inserting two electrodes into an electrolytic cell, using a platinum sheet (10 × 10 × 0.2mm) as an anode and a graphite rod (I ═ 6mm) as a cathode, and introducing 6mA of constant current to perform electrochemical reaction for 6 hours; the molar volume ratio of the catalyst to the mixture is 0.075 mol/L;
(3) after the reaction is finished, taking out the reaction liquid, adding the reaction liquid into a separating funnel, adding 20mL of water, stirring, extracting a water phase by using ethyl acetate, drying an organic phase by using anhydrous sodium sulfate, and finally performing column chromatography purification and separation to obtain 92.0mg of a product, namely nitrogen- (2-cyano-2- (4-fluorophenyl) ethyl) -nitrogen- (benzenesulfonyl) benzenesulfonamide (beta-cyanobenzenesulfonamide compounds), wherein the calculated product yield is 64%; the structural formula of the obtained product is shown as follows:
Figure BDA0003334841570000071
1H NMR(400MHz,Chloroform-d)δ8.02–7.92(m,4H),7.70–7.64(m,2H),7.54(dd,J＝8.6,7.3Hz,4H),7.42–7.32(m,2H),7.05(t,J＝8.6Hz,2H),4.53(dd,J＝8.6,6.8Hz,1H),4.16(dd,J＝15.4,8.6Hz,1H),3.94(dd,J＝15.4,6.8Hz,1H).13C NMR(101MHz,CDCl3)δ163.00(d,J＝247.0Hz),138.37,134.48,130.08(d,J＝8.5Hz),129.25,128.77,128.11(d,J＝3.3Hz),118.53,116.59(d,J＝21.9Hz),51.17,37.65.
example 3
A method for electrochemically synthesizing beta-cyano-bis-phenylsulfonyl imide compounds comprises the following specific steps:
(1) in a nitrogen atmosphere, 0.3mmol (40.2mg) of 4-trifluoromethylstyrene, 0.3mmol (81.9mg) of cyanobenzophenone and 0.45mmol (133.65mg) of bisbenzenesulfonylimide were charged into a 10 mL-volume diaphragm-free electrolytic cell, and then 4mL of acetonitrile was further added to the electrolytic cell and stirred for 20 minutes to dissolve the starting materials to obtain a mixture;
(2) adding electrolyte (n-Bu) to the mixture4NOAc), inserting two electrodes into an electrolytic cell, using a platinum sheet (10 × 10 × 0.2mm) as an anode and a graphite rod (I ═ 6mm) as a cathode, and introducing 5mA of constant current to perform electrochemical reaction for 8 hours; the molar volume ratio of the catalyst to the mixture is 0.075 mol/L;
(3) after the reaction is finished, taking out the reaction liquid, adding the reaction liquid into a separating funnel, adding 20mL of water, stirring, extracting a water phase by using ethyl acetate, drying an organic phase by using anhydrous sodium sulfate, and finally performing column chromatography purification and separation to obtain 101.8mg of a product of nitrogen- (2-cyano-2- (4- (trifluoromethyl) phenyl) ethyl) -nitrogen- (benzenesulfonyl) benzenesulfonamide (beta-cyanobenzenesulfonamide compounds), wherein the calculated product yield is 65%; the structural formula of the obtained product is shown as follows:
Figure BDA0003334841570000081
1H NMR(600MHz,Chloroform-d)δ7.98(d,J＝7.9Hz,4H),7.70(t,J＝7.5Hz,2H),7.67(d,J＝7.9Hz,2H),7.56(t,J＝8.1Hz,6H),4.66(t,J＝7.7Hz,1H),4.21(dd,J＝15.4,8.4Hz,1H),4.04(dd,J＝15.4,7.0Hz,1H).13C NMR(151MHz,CDCl3)δ138.15,136.22,134.61,131.41(q,J＝32.6Hz),129.29,128.86,128.77,126.51(q,J＝7.3Hz),123.69(q,J＝272.4Hz),118.04,50.83,38.16.19F NMR(376MHz,CDCl3)δ-111.89--111.97.
example 4
A method for electrochemically synthesizing beta-cyano-bis-phenylsulfonyl imide compounds comprises the following specific steps:
(1) in a nitrogen atmosphere, 0.3mmol (41.55mg) of 2-chlorostyrene, 0.5mmol (136.5mg) of cyanobenzophenone and 0.35mmol (103.95mg) of bisbenzenesulfonylimide were added to a 10 mL-volume diaphragm-free electrolytic cell, and then 5mL of acetonitrile was added to the electrolytic cell and stirred for 15 minutes to dissolve the starting materials to obtain a mixture;
(2) adding electrolyte (n-Bu) to the mixture4NOAc), inserting two electrodes into an electrolytic cell, using a platinum sheet (10 × 10 × 0.2mm) as an anode and a graphite rod (I ═ 6mm) as a cathode, and introducing 7mA of constant current to perform electrochemical reaction for 6 hours; the molar volume ratio of the catalyst to the mixture is 0.09 mol/L;
(3) after the reaction is finished, taking out the reaction liquid, adding the reaction liquid into a separating funnel, adding 20mL of water, stirring, extracting a water phase by using ethyl acetate, drying an organic phase by using anhydrous sodium sulfate, and finally performing column chromatography purification and separation to obtain 77.6mg of a product of nitrogen- (2-cyano- (2-chlorphenyl) ethyl) -nitrogen- (benzenesulfonyl) benzenesulfonamide (beta-cyanobenzenesulfonamide compounds), wherein the yield is calculated to be 53%; the structural formula of the obtained product is shown as follows:
Figure BDA0003334841570000091
1H NMR(600MHz,Chloroform-d)δ8.19–8.07(m,4H),7.73–7.67(m,2H),7.64–7.56(m,5H),7.46–7.42(m,1H),7.36(tt,J＝7.4,5.5Hz,2H),5.01(dd,J＝10.1,6.0Hz,1H),4.26(dd,J＝15.2,10.1Hz,1H),3.89(dd,J＝15.2,6.0Hz,1H).13C NMR(151MHz,CDCl3)δ138.44,134.52,133.28,130.70,130.41,130.19,130.15,129.25,128.97,128.16,118.07,48.83,36.06.
example 5
A method for electrochemically synthesizing beta-cyano-bis-phenylsulfonyl imide compounds comprises the following specific steps:
(1) in a nitrogen atmosphere, 0.3mmol (54.9mg) of 2-bromostyrene, 0.9mmol (245.7mg) of cyanobenzophenone and 1.3mmol (386.1mg) of bis-benzenesulfonylimide are added into a diaphragm-free electrolytic cell with the volume of 10mL, then 3mL of acetonitrile is added into the electrolytic cell, and stirring is carried out for 15 minutes to dissolve the raw materials, so as to obtain a mixture;
(2) adding electrolyte (n-Bu) to the mixture4NOAc), inserting two electrodes into an electrolytic cell, using a platinum sheet (10 × 10 × 0.2mm) as an anode and a graphite rod (I ═ 6mm) as a cathode, and introducing a constant current of 8mA for electrochemical reaction for 7 hours; the molar volume ratio of the catalyst to the mixture is 0.06 mol/L;
(3) after the reaction is finished, taking out the reaction liquid, adding the reaction liquid into a separating funnel, adding 20mL of water, stirring, extracting a water phase by using ethyl acetate, drying an organic phase by using anhydrous sodium sulfate, and finally performing column chromatography purification and separation to obtain 92.4mg of a product, namely, the nitrogen- (2-cyano- (2-bromophenyl) ethyl) -nitrogen- (benzenesulfonyl) benzenesulfonamide (beta-cyanobenzenesulfonamide compounds), wherein the yield of the product is calculated to be 58%; the structural formula of the obtained product is shown as follows:
Figure BDA0003334841570000111
1H NMR(600MHz,Chloroform-d)δ8.18–8.12(m,4H),7.74–7.68(m,2H),7.64(dd,J＝7.8,1.6Hz,1H),7.62–7.57(m,5H),7.42(td,J＝7.6,1.3Hz,1H),7.30–7.23(m,1H),5.01(dd,J＝10.3,6.1Hz,1H),4.25(dd,J＝15.2,10.3Hz,1H),3.90(dd,J＝15.2,6.1Hz,1H).13C NMR(151MHz,CDCl3)δ138.48,134.55,133.74,132.07,130.92,130.18,129.28,128.96,128.85,123.30,118.15,49.05,38.30.
example 6
A method for electrochemically synthesizing beta-cyano-bis-phenylsulfonyl imide compounds comprises the following specific steps:
(1) in a nitrogen atmosphere, 0.3mmol (46.2mg) of 2-vinylnaphthalene, 0.3mmol (81.9mg) of cyanobenzophenone and 0.45mmol (133.65mg) of bisbenzenesulfonimide were charged into a 10 mL-volume diaphragm-free electrolytic cell, and then 4mL of acetonitrile was further charged into the electrolytic cell and stirred for 10 minutes to dissolve the starting materials to obtain a mixture;
(2) adding electrolyte (n-Bu) to the mixture4NOAc), inserting two electrodes into an electrolytic cell, using a platinum sheet (10 × 10 × 0.2mm) as an anode and a graphite rod (I ═ 6mm) as a cathode, and introducing 5mA of constant current to perform electrochemical reaction for 8 hours; the molar volume ratio of the catalyst to the mixture is 0.075 mol/L;
(3) after the reaction is finished, taking out the reaction liquid, adding the reaction liquid into a separating funnel, adding 20mL of water, stirring, extracting a water phase by using ethyl acetate, drying an organic phase by using anhydrous sodium sulfate, and finally performing column chromatography purification and separation to obtain 104.3mg of a product of nitrogen- (2-cyano- (vinyl naphthalene) ethyl) -nitrogen- (benzenesulfonyl) benzenesulfonamide (beta-cyanobiphenylimide compounds), wherein the product yield is calculated to be 69%; the structural formula of the obtained product is shown as follows:
Figure BDA0003334841570000121
1H NMR(400MHz,Chloroform-d)δ7.96–7.83(m,6H),7.82–7.75(m,2H),7.61–7.47(m,5H),7.39(t,J＝7.9Hz,4H),4.71(t,J＝7.7Hz,1H),4.24-4.11(m,2H).13C NMR(101MHz,CDCl3)δ138.32,134.34,133.34,133.26,129.65,129.49,129.09,128.75,128.13,128.11,127.83,127.10,127.00,125.05,118.76,51.03,38.51.
the invention provides a method for directly preparing beta-cyano-bis-phenylsulfonylimide compounds by taking olefin, cyano-benzoxy ketone and bis-phenylsulfonylimide as raw materials and acetonitrile as a solvent in a nitrogen atmosphere by utilizing electrochemistry, wherein the synthesis method is green and environment-friendly, simple in synthesis steps, mild in reaction conditions, low in cost, high in product yield and not lower than 50% in yield.
The above-mentioned preferred embodiments of the present invention are provided for illustration only and not for the purpose of limiting the invention. Obvious variations or modifications of the present invention are within the scope of the present invention.

Claims (8)

1. The method for electrochemically synthesizing the beta-cyanobenzene sulfonyl imide compound is characterized in that the beta-cyanobenzene sulfonyl imide compound is obtained by taking olefin or derivatives thereof, cyanobenzophenone and dibenzene sulfonyl imide as reaction raw materials, acetonitrile as a solvent and tetrabutylammonium acetate as an electrolyte through electrochemical synthesis under the protection of inert atmosphere;
the alkene or the derivative thereof has a structural general formula shown in a formula (I);
Figure FDA0003334841560000011
in the formula R1Represents an alkyl group, an aromatic group or a derivative thereof.
2. The method for electrochemically synthesizing the beta-cyanobenzenesulfonimide compound according to claim 1, characterized by comprising the following specific steps:
(1) in a nitrogen atmosphere, adding the olefin or the derivative thereof, the cyanobenzophenone and the bis-benzenesulfonylimide into an electrolytic cell filled with the acetonitrile in proportion, and uniformly stirring to obtain a mixture;
(2) putting the electrolyte into the mixture, taking a platinum sheet as an anode and a graphite rod as a cathode, and introducing constant current to carry out electrochemical reaction;
(3) and after the reaction is finished, taking out the reaction liquid, adding water, stirring, extracting, drying and purifying to obtain the beta-cyano-bis-benzene sulfimide compound.
3. The method for electrochemically synthesizing a β -cyanobenzenesulfonylimide compound according to claim 2, wherein in the step (1), the olefin or the derivative thereof, the cyanobenzophenone, and the bisbenzenesulfonimide are reacted in a nitrogen atmosphere at a molar ratio of 1: (1-3): (1-5) to an electrolytic cell containing the acetonitrile, and stirring for 10-20 minutes to obtain a mixture.
4. The method of claim 3, wherein the molar ratio of the alkene or derivative thereof, the cyanobenzophenone, and the bisbenzenesulfonylimide is 1: 1: 1.5.
5. the method for electrochemically synthesizing a β -cyanobenzenesulfonimide compound according to claim 2 or 3, wherein the molar volume ratio of the olefin or derivative thereof to the acetonitrile in step (1) is 0.05 to 0.1 mol/L.
6. The method for electrochemically synthesizing a β -cyanobenzenesulfonimide compound according to claim 2, wherein in step (2), the electrolyte is put into the mixture, a platinum sheet is used as an anode, a graphite rod is used as a cathode, and a constant current of 5-8mA is applied to perform the electrochemical reaction for 6-8 hours.
7. The method for electrochemically synthesizing a β -cyanobenzenesulfonimide compound according to claim 2 or 6, wherein the molar volume ratio of the electrolyte to the mixture in step (2) is 0.05 to 0.1 mol/L.
8. The method for electrochemically synthesizing the beta-cyanobenzenesulfonamide compound according to claim 2, characterized in that after the reaction in the step (3) is finished, the reaction solution is taken out and added into a separating funnel, then water is added for stirring, ethyl acetate is used for extracting an aqueous phase, anhydrous sodium sulfate is used for drying an organic phase, and finally column chromatography purification and separation are carried out to obtain the beta-cyanobenzenesulfonamide compound.
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