Synthesis method of N, N-dimethyl trifluoromethanesulfonamide

A technology of dimethyltrifluoromethanesulfonamide and trifluoromethanesulfonyl fluoride, which is applied in the field of battery electrolyte additives, can solve the problems of harsh conditions, poor purity, and low reaction yield, and achieve a mild reaction process, Increased yield and simple reaction process

Pending Publication Date: 2021-12-17
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, the preparation process of N,N-dimethyltrifluoromethanesulfonamide mainly generates N,N-dimethyltrifluoromethanesulfonamide through the reaction of trifluoromethanesulfonamide and methyl halide, the shortcoming of this reaction Yes, the conditions required for the reaction process are

Method used

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  • Synthesis method of N, N-dimethyl trifluoromethanesulfonamide
  • Synthesis method of N, N-dimethyl trifluoromethanesulfonamide
  • Synthesis method of N, N-dimethyl trifluoromethanesulfonamide

Examples

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Example Embodiment

[0020] Example 1:

[0021] Synthesis of N, N-dimethyl triflicalasulfonamide, the synthesis steps are as follows:

[0022] Add 16.91 g (0.15 mol) concentration of 40 wt% dimethylamine aqueous solution to the high pressure reactor, cool down to 5 ° C, slowly drop 15.2 g (0.1 mol) trifluorometacyl fluoride, then add it, then add 8.1 g (0.08 mol) triethylamine, then elevated pressure to 0.5 MPa, maintaining 0.5 MPa temperature rise to 20 ° C for an amidation reaction for 20 h, after the amidation reaction, concentrated, then ether as a column chromatography Purification, collected, concentrated elution, concentrated under reduced pressure, 15.89 g of N, N-dimethyltrodunnesulfonamide, yield 89.70%, purity 99.5%, and the specific chemical reaction is as follows:

[0023]

Example Embodiment

[0024] Example 2:

[0025] Synthesis of N, N-dimethyl trifluoromethanesulfonamide, the synthesis steps are as follows

[0026] Take 19.16 g (0.17 mol) concentration of 40 wt% dimethylamine aqueous solution to the high pressure reaction kettle, cool down to 0 ° C, slowly drop 15.2 g (0.1 mol) trifluorometacyl fluoride, then add it, add 7.08 g (0.07 mol) triethylamine, then elevated to 0.1 MPa, maintaining 0.1 MPa heating to 15 ° C for an amidation reaction for 22 h, after the amidation reaction was completed, then concentrated, and then evaporation was chromatography Purification, collected, concentrated elution, concentrated under reduced pressure, 15.64 g of N, N-dimethyltrodunnesulfonamide, yield 88.29%, purity 99.6%.

Example Embodiment

[0027] Example 3:

[0028] Synthesis of N, N-dimethyl triflicalasulfonamide, the synthesis steps are as follows:

[0029] EtOAc. 6.07 g (0.06 mol) triethylamine, then elevated pressure to 0.3 MPa, maintaining 0.3 MPa heating to 10 ° C for an amidation reaction for 20 h, after the amidation reaction was completed, then concentrated, then evaporation was chromatography Purification, collected, concentrated elution, concentrated under reduced pressure, 15.73 g of N, N-dimethyltrodunnesulfonamide, yield of 88.79%, purity 99.6%.

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Abstract

The invention discloses a synthesis method of N, N-dimethyl trifluoromethanesulfonamide, and relates to the technical field of battery electrolyte additives, and the synthesis method comprises the following steps: taking trifluoromethanesulfonyl fluoride and dimethylamine, and carrying out amidation reaction under the condition of 0.1-0.5 MPa to obtain the N, N-dimethyl trifluoromethanesulfonamide. The preparation method comprises the following steps: taking trifluoromethanesulfonyl fluoride and dimethylamine as raw materials, and directly carrying out amidation reaction; the reaction process is simple, raw materials used in the reaction are easy to obtain, the reaction process is milder and safer compared with the prior art, the product yield and product purity maximization in the production process are guaranteed through control over reaction conditions in all stages, the product yield is further increased by reasonably controlling the use amount of the reaction raw materials and the reaction process, the yield reaches 88.29% or above, and the purity reaches 99.5% or above.

Description

technical field [0001] The invention relates to the technical field of battery electrolyte additives, in particular to a synthesis method of N,N-dimethyltrifluoromethanesulfonamide. Background technique [0002] Lithium-ion batteries are currently the most common electrical energy storage devices. Compared with traditional batteries, they have higher storage capacity and more stable performance. The key factors affecting the performance of lithium-ion batteries lie in the performance of organic electrolytes. In battery production, an electrolyte additive containing N,N-dimethyltrifluoromethanesulfonamide is added to the electrolyte to increase the concentration of hydrogen ions in the electrolyte and reduce the loss in the process of electric energy conversion. [0003] In the prior art, the preparation process of N,N-dimethyltrifluoromethanesulfonamide mainly generates N,N-dimethyltrifluoromethanesulfonamide through the reaction of trifluoromethanesulfonamide and methyl hal...

Claims

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Application Information

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IPC IPC(8): C07C303/38C07C311/09
CPCC07C303/38C07C311/09
Inventor 林胜赛李庆占邢艳召刘鹏田丽霞张茜张民彭鹏鹏郝俊侯荣雪王军葛建民武利斌闫彩桥许晓丹闫朋飞杨世雄赵光华高山
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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