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Alkylviolagen iodine salt preparation method

A technology of violet essence and iodized salt, applied in organic chemistry and other directions, can solve problems such as human body and environmental impact, and achieve the effects of no environmental impact, reduced pollution, and high purity

Inactive Publication Date: 2008-01-30
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are many patents (CN1226554A, CN 1228425A) disclosing improvements to minimize the cyanide residue in the product, it is still necessary to use highly toxic alkali metal cyanide as a catalyst, which has an impact on the human body and the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Weigh 3mmol of 4,4-bipyridine into the autoclave, then add methyl iodide in a molar ratio of 1:2, mix well, add 2ml of methanol, seal the autoclave, and dry it at a constant temperature In the box, at the set temperature of 100°C, the reaction was carried out at constant temperature for 5 hours. Take out the autoclave, wait for it to cool down naturally, open it, let excess methyl iodide volatilize, and dry it at room temperature to obtain methyl viologen iodide salt. When calculating the yield with 4,4-bipyridine as the reactant, the yield of methyl viologen iodide salt is higher than 95%.

Embodiment 2

[0015] Weigh 5mmol of 4,4-bipyridine into the autoclave, then add ethyl iodide in a molar ratio of 1:5, mix well, add 6ml of methanol, seal the autoclave, and place it at a constant temperature In a drying oven, at a set temperature of 130° C., a constant temperature reaction was carried out for 4.5 hours. Take out the autoclave, wait for it to cool down naturally, open it, let excess iodoethane volatilize, and dry it at room temperature to obtain ethyl viologen iodized salt. When the yield is calculated with 4,4-bipyridine as the reactant, the yield of ethyl viologen iodide is greater than 95%.

Embodiment 3

[0017] Weigh 4mmol of 4,4-bipyridine into the autoclave, add iodopropane in a molar ratio of 1:6, mix well, add 8ml of methanol, seal the autoclave, and put it in a constant temperature drying box Here, at a set temperature of 120°C, the reaction was carried out at a constant temperature for 3.5 hours. Take out the autoclave, wait for it to cool down naturally, open it, let the excess iodopropane volatilize, and dry it at room temperature to obtain propyl viologen iodide salt. When calculating the yield with 4,4-bipyridine as the reactant, the yield of the iodized alkyl viologen salt is above 95%.

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PUM

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Abstract

The present invention is alkyl violagen iodine salt preparing process. The preparation process includes mixing 4, 4-dipyridine and iodic alkane in the molar ratio of 1 to 2-8, setting the mixture into high pressure reactor, adding methanol, sealing the high pressure reactor and setting it into drying case, reaction at 100-150 deg.c for 2-6 hr, taking out the high pressure reactor, cooling naturally, opening the high pressure reactor, volatilizing excessive iodic alkane, and drying in the air to obtain alkyl violagen iodine salt. The present invention adopts no toxic catalyst, and has no environmental pollution, high product purity up to 95 %, simple technological process and short reaction period.

Description

technical field [0001] The invention relates to the technical field of synthesis of fine chemicals, in particular to a method for preparing alkyl viologen iodide salts with different alkyl chains. Background technique [0002] In recent years, bipyridyl has been widely used in the production of herbicides, and is also an intermediate in the production of pharmaceuticals and organic chemical raw materials. Alkyl viologen iodide salt is an important photocatalyst and a quick-acting contact herbicide, which is quickly inactivated after contacting the soil, has no residue in the soil, and will not damage the roots of plants, so it can be applied to a variety of crops , to help increase agricultural production. The traditional method of synthesizing alkyl viologen iodide salt is to use alkali metal cyanide to catalyze the coupling of 1-alkylpyridinium salt, and then oxidize it. However, the product often does not meet the requirements because the residual cyanide and inorganic ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/22
Inventor 单永奎赖克强王一蕾孔爱国顾颖颖
Owner EAST CHINA NORMAL UNIV