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Preparation method of 2-chloropyridine n-oxides

A technology of chloropyridine nitrogen oxide and chloropyridine, which is applied in the direction of organic chemistry, can solve the problems of many by-products, long reaction time of sodium perborate, and large amount of peroxide, so as to improve conversion rate, simple operation process, The effect of small investment in equipment

Active Publication Date: 2014-08-20
NANTONG ACETIC ACID CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In the peroxide oxidation method, the amount of peroxide used is large, and cannot be fully utilized, such as "Study on the Synthesis of 2-Chloropyridine Nitrogen Oxide" (Zheng Shuling et al., Journal of Tianjin Normal University, 2006, 26 (1): 9 -11),; Sodium perborate has a long reaction time, poor reaction selectivity, many by-products, and complex post-processing

Method used

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Examples

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Embodiment 1

[0036] Dissolve 25g of trimethylhexadecylammonium bromide in 200ml of deionized water, keep stirring at 20-60°C for 30 minutes, add 50g of Na 2 SiO 3 , stir well, use dilute H 2 SO 4 The pH of the solution was adjusted to 8.5, then 60 ml of an aqueous solution containing 7.5 g of titanium trichloride was added dropwise to the above solution under vigorous stirring, and 220 ml of an aqueous sodium stannate solution containing 30.0 g of sodium stannate trihydrate was added dropwise, and Ammonia water was adjusted to pH 9.0~9.5, and finally 40 ml of an aqueous solution containing 19.0 g of sodium tungstate dihydrate was added. The obtained mixed sol was stirred for 2 hours, then transferred to a stainless steel autoclave, and hydrothermally reacted at 120 °C for 24 hours. After the reaction, the mixture was cooled to room temperature with water, and the product was filtered, washed three times with deionized water and anhydrous ethanol, and dried at room temperature. The origi...

Embodiment 2

[0038] Dissolve 25g of trimethylhexadecylammonium bromide in 200ml of deionized water, keep stirring at 20-60°C for 30 minutes, add 50g of Na 2 SiO 3 , stir well, use dilute H 2 SO 4 The pH of the solution was adjusted to 8.5, then 40 ml of an aqueous solution containing 5 g of titanium trichloride was added dropwise to the above solution under strong stirring, and 150 ml of an aqueous sodium stannate solution containing 20.0 g of sodium stannate trihydrate was added dropwise, and ammonia water was used. Adjust the pH to 9.0~9.5, and finally add 25 ml of an aqueous solution containing 12.7 g of sodium tungstate dihydrate. The obtained mixed sol was stirred for 2 hours, then transferred to a stainless steel autoclave, and hydrothermally reacted at 120 °C for 24 hours. After the reaction, the mixture was cooled to room temperature with water, and the product was filtered, washed three times with deionized water and anhydrous ethanol, and dried at room temperature. The origina...

Embodiment 3

[0040] Dissolve 25g of trimethylhexadecylammonium bromide in 200ml of deionized water, keep stirring at 20~60°C for 30 minutes, add 50g of Na2SiO3 to it, stir evenly, adjust the pH of the solution to 8.5 with dilute H2SO4, and then add 50g of Na2SiO3 to it. Under stirring, 20ml of an aqueous solution containing 2.5g of titanium trichloride was added dropwise to the above solution, and then 50ml of an aqueous solution of sodium stannate containing 13.7g of sodium stannate trihydrate was added dropwise, and the pH was adjusted to 9.0~9.5 with ammonia water. 15 ml of an aqueous solution of 8.5 g of sodium tungstate dihydrate. The obtained mixed sol was stirred for 2 hours, then transferred to a stainless steel autoclave, and hydrothermally reacted at 120 °C for 24 hours. After the reaction, the mixture was cooled to room temperature with water, and the product was filtered, washed three times with deionized water and anhydrous ethanol, and dried at room temperature. The original ...

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Abstract

The invention discloses a preparation method of 2-chloropyridine n-oxides. According to the preparation method, 2-chloropyridine and catalytic agents are mixed according to a mass ratio of 1 : (0.05-0.5), the 2-chloropyridine and the catalytic agents are stirred at the temperature between 40 DEG C and 90 DEG C, and hydrogen peroxide is added for reaction; the temperature is kept unchanged, the mixture is stirred for performing reaction for 3-10 hours, then the temperature is lowered to a normal temperature, and after the reaction, the mixture is filtered to obtain a 2-chloropyridine n-oxide water solution; the molar ratio between the hydrogen peroxide and the 2-chloropyridine is (0.8-3.5) : 1; and the catalytic agents use mesoporous molecular sieves (MCM-41) as carriers. Under the actions of the high-activity and high-selectivity catalytic agents, the 2-chloropyridine is reacted with the hydrogen peroxide to obtain the 2-chloropyridine n-oxides, the reaction conversion ratio of the 2-chloropyridine reaches 100%, and the yield of the 2-chloropyridine n-oxides reaches above 98%.

Description

technical field [0001] The invention relates to a preparation method of a heterocyclic compound, in particular to a preparation method of 2-chloropyridine nitrogen oxide. Background technique [0002] 2-Chloropyridine nitrogen oxide, its molecular formula and molecular weight: C 5 H 4 ClNO=129.5 [0003] Physical and chemical properties: This product is white crystal, the aqueous solution is amber, easily deliquescence, soluble in water, alcohol, slightly soluble in ether. Melting point: 67-70℃, Boiling point: 168-170℃, Density: 1.209g / cm 3 , Refractive Index: 1531-1533. [0004] Function and use: It is an important compound in the pyridine series nitrogen oxides, an important intermediate of pesticides, medicines and daily chemical products, and it is also an anti-corrosion and anti-corrosion agent for the synthesis of skin cleansers, shampoos and pyrithione. It is an important intermediate of mold fungicides and an essential raw material for the synthesis of 2-chloro-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/89
Inventor 丁彩峰林民朱小刚刘芳吴慰祖舒兴田周新建薛建锋王健华朱双双
Owner NANTONG ACETIC ACID CHEM
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