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Ternary sulfonimine alkali salt and synthesis method thereof

A technology of sulfonimide base and synthesis method, which is applied in the field of ternary sulfonimide alkali metal salt and its synthesis, and achieves the effects of superior electrochemical stability and good electrical conductivity

Inactive Publication Date: 2005-11-16
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But its synthetic steps are daunting

Method used

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  • Ternary sulfonimine alkali salt and synthesis method thereof
  • Ternary sulfonimine alkali salt and synthesis method thereof
  • Ternary sulfonimine alkali salt and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1: Utilize sulfonamide sodium salt to synthesize aliphatic fluorine-containing tribasic sulfonylimide sodium nitrate

[0036]

[0037] Synthetic steps:

[0038]

[0039] solvent

a

b

c

Yield

CH 3 NO 2

CH 3 CN

0.014

0.015

0.0028

0.0030

1.82

2.00

81％

83％

[0040] Structure Characterization:

[0041] FT-IR: 3000cm -1 There is no N-H vibration above, and there are obvious water peaks. The fingerprint area is also obviously different from the raw material, 995, 800, 700, 500cm in the raw material -1 The absorption peak at the point disappears in the product.

[0042] 1 H NMR: (TMS internal standard, DMSO-d 6 for the solvent) 1 The H NMR spectrum shows that there is no H atom in the compound, indicating that it does not contain raw materials and other H-containing impurities.

[0043] 19 F NMR: (CFCl 3 Internal standard, DMSO-d 6 is the solvent) has the fol...

Embodiment 2

[0048] Example 2: Utilize fluorine-containing sulfonamide to synthesize fluorine-containing ternary sulfonylimide sodium nitrate

[0049] (1) Synthesis of fluorine-containing ternary sulfonylimide nitric acid

[0050] Synthetic steps

[0051]

[0052] solvent

a

b

c

Yield

CH 3 NO 2

CH 3 CN

0.0081

0.0108

0.0162

0.0216

1.10

1.59

18％

20％

[0053] Structure Characterization:

[0054] FT-IR: 3120cm -1 There is a single N-H stretching vibration, with C 4 f 9 SO 2 NH 2 The comparison found that the characteristic peaks (946, 800, 655, 500cm) of many raw materials in the fingerprint area -1 )disappear

[0055] 1 HNMR: (TMS internal standard, DMSO-d 6 For solvent) there are three equal-area peaks at 6.46, 7.04, and 7.60ppm, which are triplets formed by H-N coupling, 1 J HN = 56Hz. No C in the spectrum 4 f 9 SO 2 NH 2 H peak (7.52ppm).

[0056] 19 F NMR: (CFCl 3 Interna...

Embodiment 3

[0063] Embodiment 3: Utilize sulfonamide sodium salt to synthesize ternary sodium sulfonimide nitrogen superacid with aromatic ring

[0064] Synthetic steps:

[0065]

[0066] solvent

a

b

c

Yield

CH 3 NO 2

CH 3 CN

0.0200

0.0168

0.0040

0.0034

2.05

1.54

70％

75％

[0067] Structure Characterization:

[0068] FT-IR: compared with sodium p-nitrobenzenesulfonamide, 990cm -1 The strong peak at disappears, and the fingerprint area is obviously different, 3300cm in the raw material -1 The peak disappears

[0069] 1 H NMR: (TMS internal standard, DMSO-d 6 There are symmetrical multiple peaks at 7.66-8.04ppm, which is the solvent, and it is a para-substituted aromatic H, and no active hydrogen peaks are found in the amine group

[0070] Elemental analysis: C (23.12%, ca.23.57%), N (11.07%, ca.11.46%), H (1.93%, ca.1.31%)

[0071] Melting point: 270°C turns black

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Abstract

The present invention discloses a ternary sulfonylimine alkali metal salt and its synthesis method. Said invention provides its structure general formula, and its synthesis method includes the following steps: using anhydrous strong-polarity solvent to dissolve 5 portions of sulfamine salt, drop-adding the solution containing 1 portion of dichlorosulfimine into said system to make reflux reaction, when the precipitate is not increased, stopping said reaction to obtain lots for precipitate, cooling, standing still and filtering, and dissolving said precipitate by using a certain quantity of anhydrous strong-polarity solvent, refluxing, filtering, drying the solid under the condition of reducing pressure to obtain end product.

Description

technical field [0001] The invention relates to a sulfonylimide compound, in particular to a ternary sulfonylimide alkali metal salt and a synthesis method thereof. The alkali metal salt has good electrical conductivity and electrochemical stability. Background technique [0002] A lot of work has been done on the research on sulfonimide nitrogen superacids and their metal salts, and many important results have been obtained. This can be mainly divided into two aspects: the application of sulfonimide nitrogen superacid transition metal salts (especially lanthanide metal salts) in organic synthesis as efficient Lewis acid catalysts; Or the application of alkaline earth metal salts in liquid electrolytes and solid electrolytes. [0003] The excellent properties and broad application prospects of these compounds attract chemists to continuously devote themselves to the development of new structural nitrogen superacids and their derivatives. However, most studies have focused...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C311/48C07C381/00C07F5/00
Inventor 聂进李小永张正波
Owner HUAZHONG UNIV OF SCI & TECH
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