Method for preparing nitrogen-containing onium salt compounds

A nitrogen compound and compound technology are applied in the field of preparation of nitrogen-containing onium salt compounds, which can solve the problems of high toxicity of halogenated hydrocarbons, insufficient variety of nitrogen-containing onium salt compounds, etc., and achieve low toxicity, simple method and wide source of raw materials. Effect

Inactive Publication Date: 2008-02-13
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the toxicity of halogenated hydrocarbons is relatively large, and, being limited by the type of halogenated hydrocarbons, the types of nitrogen-containing onium salt compounds obtained are not abundant enough.

Method used

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  • Method for preparing nitrogen-containing onium salt compounds
  • Method for preparing nitrogen-containing onium salt compounds
  • Method for preparing nitrogen-containing onium salt compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment one: referring to accompanying drawing 1, a kind of preparation method of nitrogen-containing onium salt compound comprises the following steps:

[0038] (1) Add 0.1 mmol of cuprous iodide (CuI), 0.1 mmol of iodine (I 2 ), 0.1 mmol 4,4'-bipyridine and 1 milliliter of ethanol are reaction initiators, mixed in 1 milliliter of acetonitrile, and reacted for 70 hours under solvothermal reaction conditions;

[0039] (2) Then, the temperature is gradually lowered at a rate of 5°C per 100 minutes to obtain black needle-like crystals with a single crystal structure {[C 14 h 18 N 2 ][Cu 2 I 4 ]} n As shown in Figure 1, the ethyl group on ethanol is transferred to the N of 4,4′-bipyridyl to form an onium cation [C 14 h 18 N 2 ] 2+ , the polyanion is one-dimensional (Cu 2 I 4 ) n 2n- chain.

[0040] (3) Pour acetonitrile into the precipitated mixture, stir, stop stirring, and pour it when the product crystals precipitate and the impurities do not precipitate,...

Embodiment 2

[0042] Embodiment two: referring to accompanying drawing 2, a kind of preparation method of nitrogen-containing onium salt compound comprises the following steps:

[0043] (1) 0.05 mmol of cuprous iodide, 0.05 mmol of iodine, 0.05 mmol of 4,4'-dipyridine and 0.5 milliliter of n-propanol are used as reaction starting materials, mixed in 1.5 milliliters of acetonitrile, and reacted in solvothermal Reaction under the conditions for 70 hours;

[0044] (2) Then gradually lower the temperature gradually at a rate of 5°C every 65 minutes to obtain black needle-like crystals with a single crystal structure {[C 16 h 22 N 2 ][Cu 2 I 4 ]} n As shown in Figure 2, the propyl group on n-propanol is transferred to the N of 4,4′-bipyridine to form an onium cation [C 16 h 22 N 2 ] 2+ , the polyanion is one-dimensional [Cu 2 I 4 ] n 2n- chain.

[0045] (3) The separation and purification process is the same as step (3) of Example 1. Yield: 83.11%.

[0046] (4) Elemental analysis...

Embodiment 3

[0047] Embodiment three: referring to accompanying drawing 3, a kind of preparation method of nitrogen-containing onium salt compound comprises the following steps:

[0048] (1) 0.1 mmol of cuprous iodide, 0.1 mmol of iodine, 0.1 mmol of 4,4'-bipyridine and 1 ml of isopropanol were used as reaction starting materials, mixed in 1 ml of acetonitrile, and reacted in solvothermal Reaction under the conditions for 70 hours;

[0049] (2) Then gradually lower the temperature at a rate of 5°C every 100 minutes to obtain dark brown flaky crystals with a single crystal structure [C 16 h 22 N 2 ][CuI 3 ] As shown in Figure 3, the isopropyl group on the isopropanol is transferred to the N of 4,4'-bipyridine to form an onium cation [C 16 h 22 N 2 ] 2+ , with anion [CuI 3 ] 2- .

[0050] (3) The separation and purification process is the same as step (3) of Example 1. Yield: 79.45%.

[0051] (4) Elemental analysis: theoretical value (C 16 h 22 N 2 CuI 3 ): C, 27.99; H, 3.23;...

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Abstract

The invention discloses a method for preparing an onium salt compound: taking iodine simple substance, metal iodide, alcohol and a nitrogen-containing compound, mixing them in acetonitrile, and reacting for several hours under solvothermal conditions to generate a single crystal of the onium salt compound in situ. The method has strong applicability, wide source of raw materials, cheap and easy to obtain, high product purity and yield, simple reaction device, simple method, and no inert gas protection is needed in the reaction process.

Description

technical field [0001] The present invention relates to a method for preparing a nitrogen-containing onium salt compound, and the present invention also relates to the use of the onium salt compound synthesized by the method. Background technique [0002] Nitrogen-containing onium salt compounds play a decisive role in people's production and life. In the prior art, common uses of such compounds include: [0003] 1. Phase transfer catalyst. In the field of organic synthetic chemistry, nitrogen-containing onium salt compounds are very important phase transfer catalysts. Phase transfer catalysis (PTC) was developed in the early 1970s. Since Cassar first used phase transfer catalysts and transition metal complexes in 1976 to catalyze organic synthesis reactions (Cassar, L., Foa, M., Gardano, A., J.Organoment.Chem.1976, 121 (3), C55), this method has obtained rapid development in recent years, has been widely used in reactions such as oxidation, reduction, carbonylation, coupl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/22C07D213/24C07D401/14
Inventor 郎建平陈阳任志刚李红喜
Owner SUZHOU UNIV
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