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Method for preparing sulfimide compound

A technology of sulfonimide salt compound and sulfonamide, applied in the preparation of sulfonamide, organic chemistry and other directions, can solve the problems of high price of trifluoromethanesulfonamide, difficulty in large-scale production, unsuitable for mass production, etc. Low cost, ease of operation, improved purity and yield

Inactive Publication Date: 2011-03-09
SHANGHAI SINOFLUORO SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, because the raw material trifluoromethanesulfonamide used in the first step is expensive, and trifluoromethanesulfonyl fluoride is a highly corrosive gas, a high-pressure reactor with special materials is required and the operation is very difficult, so this method is not suitable. for mass production
[0006] As mentioned above, the current preparation technology requires special equipment and uses expensive raw materials, the cost is high, and it is difficult to produce on a large scale in industrial production

Method used

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  • Method for preparing sulfimide compound
  • Method for preparing sulfimide compound
  • Method for preparing sulfimide compound

Examples

Experimental program
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Effect test

Embodiment 1

[0024]

[0025]

[0026] CF 3 SO 2 NH 2 Synthesis:

[0027] After taking 1000mL of liquid ammonia, add 250mL of CF dropwise with a constant pressure dropping funnel 3 SO 2Br, a yellow substance was formed, the dropwise addition was completed in 1h, and the reaction was stopped after 3h to obtain a light yellow solid, and then the excess ammonia was allowed to volatilize naturally at room temperature. Prepare 50% sulfuric acid solution and adjust the pH=2 of the system. Then add 500mL of refined acetonitrile, shake to dissolve, then filter with suction, and wash twice with 150mL of acetonitrile. Acetonitrile was distilled off under reduced pressure to obtain a slightly yellow waxy solid.

[0028] CF 3 SO 2 NH 2 Refined:

[0029] CF will be produced 3 SO 2 NH 2 Recrystallize with refined toluene, use a reflux device, heat until it is completely dissolved when boiling, and precipitate crystals after cooling, obtain the product by suction filtration, dry and sto...

Embodiment 2

[0033] (CF 3 SO 2 ) 2 Synthesis of NLi:

[0034]

[0035] Take the refined CF 3 SO 2 NH 2 (7.5g, 50mmol) was added to a 500mL three-necked flask, then 200mL tributylamine was added to dissolve, heated to 35°C, CF 3 SO 2 NH 2 All dissolved. Use a pipette to measure 8 mL of CF 3 SO 2 Add Br to the dropping funnel, slowly add CF dropwise 3 SO 2 Br, the temperature was kept at 30°C, and the dropwise addition was completed in 1 hour, and the color of the solution gradually changed from reddish brown to dark red. Keep the reaction at 70°C for 6h, then distill off the solvent tributylamine under reduced pressure, and dissolve the residue in CH 2 Cl 2 , washed 3 times with water, then washed with anhydrous MgSO 4 The organic phase in the lower layer was dried, filtered with suction and then concentrated by vacuum distillation with a water pump to obtain a dark red oily substance. in N 2 Dissolve the obtained dark red oil with 250mL of methanol under protection, add...

Embodiment 3

[0038] Take the refined CF 3 SO 2 NH 2 (7.5g, 50mmol) was added to a 500mL three-necked flask, then 250mL triethylamine was added, heated to 50°C, CF 3 SO 2 NH 2 All dissolved. Measure 12mL of CF 3 SO 2 Add Br to the dropping funnel, slowly add CF dropwise 3 SO 2 Br, the temperature was kept at 50°C, and the dropwise addition was completed in 60 minutes, and the color of the solution gradually changed from reddish brown to dark red. Then the temperature is raised to 70°C, in order to make the CF 3 SO 2 NH 2 Fully reacted, add 1mL CF after 4h 3 SO 2 Br, and then reacted for 4h. Then evaporate the solvent on the rotary evaporator, the temperature of the water bath is 50 ° C, and the dark red oil remains, and the residue is dissolved in 200 mL CH 2 Cl 2 , washed 3 times with water, separated the lower CH 2 Cl 2 , with anhydrous MgSO 4 After drying and suction filtration, the product was distilled and concentrated under reduced pressure with a water pump to obta...

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Abstract

The invention provides a method for preparing a sulfimide compound as shown in the formula (1): MN(SO2CF3) (SO2CF3), wherein M represents H and IA group alkali metals. The sulfimide compound utilizes bromotrifluoromethane easily obtained in industrial production as a raw material, and is prepared by the steps of sulfinatodehalogenation, bromination and ammoniation. The method can be used for organic synthesis, has high purity and yield as well as low cost, and can solve the problem that the sulfimide compound is difficult to realize large-scale application in industrial production due to high cost.

Description

technical field [0001] The present invention relates to a kind of formula (I) MN (SO 2 CF 3 )(SO 2 CF 3 ) The preparation method of the sulfonylimide salt compound represented. Background technique [0002] The sulfonimide salt compound can be used as a lithium battery electrolyte, and the lithium battery electrolyte using the sulfonimide salt compound as a solute has high energy density, high stability and conductivity. Therefore, sulfonylimide salts are considered to be a good solute for lithium battery electrolytes. At the same time, the sulfonylimide salt compound can also be used as a Lewis acid catalyst and ion conducting agent. Among them, among these sulfonylimide salt compounds, bis-trifluoromethanesulfonylimide lithium (CF 3 SO 2 ) 2 NLi is the most widely used one. [0003] But in the present preparation formula (I) MN (SO 2 CF 3 )(SO 2 CF 3 ) on behalf of the sulfonylimide salt compound method, there are low yield and high cost, not suitable for mass...

Claims

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Application Information

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IPC IPC(8): C07C311/48C07C303/38
Inventor 刘慧敏张巍
Owner SHANGHAI SINOFLUORO SCI
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