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Oxosynthesis method of methylpyridine-1-oxide

A technology for methyl pyridine nitrogen oxide and oxidative synthesis, which is applied in the direction of organic chemistry and the like, can solve the problems of complex catalyst preparation process, low production efficiency, and high preparation cost, and achieves low use cost, less use amount, and simple preparation process. Effect

Active Publication Date: 2015-10-28
NANTONG ACETIC ACID CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0019] The object of the present invention is to provide a kind of oxidative synthesis method of picoline nitrogen oxide in view of the shortcomings of low production efficiency, complex process, complex catalyst preparation process and high preparation cost in the existing preparation process of picoline nitrogen oxide. Catalyst preparation is simple, reaction conversion rate, product yield and product purity are high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) Preparation of catalyst

[0040] ① Weigh 10g of activated carbon (AC), wash it with tap water several times until the lotion is clear, then boil it with distilled water at high temperature for 1 hour, then filter out the liquid, repeat the above cleaning and high temperature boiling process for 5 times, and then put the activated carbon into the oven for 90 Dry at ℃ for 3 hours, cool to room temperature and set aside;

[0041] ②Accurately weigh 1g of phosphotungstic acid (TPA) and dissolve it in deionized water. After the TPA is completely dissolved, add 2.5g of the pretreated activated carbon in step ①, stir until it is completely wetted, and ultrasonically treat for 5 minutes at a power of 50W, then take out the activated carbon After continuing to stir the mixture with phosphotungstic acid solution, treat it with ultrasonic waves for 5 minutes, take out the mixture of activated carbon and phosphotungstic acid solution, and evaporate the solvent to obtain activate...

Embodiment 2

[0046] (1) Preparation of catalyst

[0047] ① Weigh 10g of activated carbon, wash it with tap water several times until the lotion is clear, then boil it with distilled water at high temperature for 1 hour, then filter out the liquid, repeat the above cleaning and high temperature boiling process for 3 times, and then put the activated carbon in an oven at 95°C to dry for 3 hours , after cooling for later use;

[0048] ② Accurately weigh 1g of phosphotungstic acid (H 3 o 40 PW 12 .xH 2 O) Dissolve in deionized water, after the phosphotungstic acid is completely dissolved, add 2g of the pretreated activated carbon in step ①, stir carefully until completely wetted, under 100W power, ultrasonic treatment for 8min, take out the mixture of activated carbon and phosphotungstic acid solution After continuing to stir, use ultrasonic treatment for 8 minutes, take out the mixture of activated carbon and phosphotungstic acid solution, evaporate and remove the solvent to obtain activa...

Embodiment 3

[0053] (1) Preparation of catalyst

[0054] ①Weigh 10g of activated carbon, wash it several times with tap water until the lotion is clear, then boil it with distilled water at high temperature for 1 hour, then filter out the liquid, repeat the above cleaning and high temperature boiling process twice. Put the activated carbon in an oven to dry at 80°C for 2 hours, and then set aside after cooling;

[0055] ②Accurately weigh 1g of phosphotungstic acid and dissolve it in deionized water. After the phosphotungstic acid is completely dissolved, add 3g of the pretreated activated carbon in step ① as a carrier, stir carefully until it is completely wetted. After the mixture of activated carbon and phosphotungstic acid solution was continuously stirred, it was treated with ultrasonic waves for 6 minutes, the mixture of activated carbon and phosphotungstic acid solution was taken out, and the solvent was evaporated to obtain the activated carbon-supported phosphotungstic acid catalys...

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Abstract

The invention discloses an oxosynthesis method of methylpyridine-1-oxide, comprising two steps of preparation of a catalyst and oxidation reaction, wherein the preparation of the catalyst comprises the steps of after cleaning, high temperature boiling, drying and cooling pretreatment of activated carbon, adding into a phosphotungstic acid solution, stirring till complete soaking, and after ultrasonic treatment, evaporating to remove a solvent to obtain a phosphotungstic acid supported on active carbon catalyst; the oxidation reaction comprises the steps of mixing methylpyridine with the phosphotungstic acid supported on active carbon catalyst, stirring, adding hydrogen peroxide for reaction, and separating the phosphotungstic acid supported on active carbon catalyst to obtain methylpyridine-1-oxide filtrate being a methylpyridine-1-oxide crude product, and distilling under reduced pressure to obtain the product. When the method is used for preparing the catalyst, a carrier is cheap and convenient, a preparation process is simple, the catalyst in the oxidation reaction is less in use level, convenient to recycle, resuable and low in cost, product yield is up to 97%, product purity is up to 98% and productivity is more than 98%.

Description

technical field [0001] The invention belongs to the field of fine organic synthesis, and in particular relates to an oxidation synthesis method of picoline nitrogen oxide. Background technique [0002] Pyridine nitrogen oxide is the collective name of 2-picoline nitrogen oxide, 3-picoline nitrogen oxide and 4-picoline nitrogen oxide, and its molecular formula is C 6 h 7 NO, molecular weight 109.3. in: [0003] (1) 2-methylpyridine nitrogen oxide [0004] English name: 2-methyl-pyridin 1-oxide [0005] CAS: 931-19-1 [0006] Physical properties: white crystal, melting point 46-50°C, boiling point 259-261°C, flash point 143°C, soluble in water. [0007] (2) 3-methylpyridine nitrogen oxide [0008] English name: 3-methylpyridine-1-oxide [0009] CAS: 1003-73-2 [0010] Physical properties: white crystal, melting point 38-40°C, boiling point 150°C (15 mmHg), flash point 143°C, soluble in water. [0011] (3) 4-methylpyridine nitrogen oxide [0012] English name: 4-meth...

Claims

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Application Information

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IPC IPC(8): C07D213/89
CPCC07D213/89
Inventor 朱蓓蓓周杰何晓春
Owner NANTONG ACETIC ACID CHEM
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