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2-acetylpyridine isonicotinic acid hydrazide molybdenum complex and preparation method thereof

A technology of acetylpyridine and isoniazid is applied in chemical instruments and methods, compounds containing elements of Group 6/16 of the periodic table, organic compounds/hydrides/coordination complex catalysts, etc. Molybdenum Schiff base complex and other problems, to achieve the effect of excellent catalytic performance, mild reaction conditions and simple operation

Active Publication Date: 2016-04-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But so far, there are no reports of molybdenum Schiff base complexes

Method used

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  • 2-acetylpyridine isonicotinic acid hydrazide molybdenum complex and preparation method thereof
  • 2-acetylpyridine isonicotinic acid hydrazide molybdenum complex and preparation method thereof
  • 2-acetylpyridine isonicotinic acid hydrazide molybdenum complex and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Weigh 10 mmol of isoniazid, put it into a round-bottomed flask (50 ml) containing 20 ml of absolute ethanol, heat and stir at 50° C., add 10 mmol of 2-acetylpyridine after the isoniazid is completely dissolved, After stirring for 1 hour, let it stand still. After 7 days, the white needle-like crystals were separated by suction filtration, and washed with a small amount of ethanol to obtain 2-acetylpyridine isonicotinoid hydrazide Schiff base complex.

[0019] Weigh 5mmol of 2-acetylpyridine isoniazid Schiff base complex, put it into a round-bottomed flask (50ml) containing 15ml of absolute ethanol, heat and stir at 75°C, and wait until 2-acetylpyridine isoniazid After completely dissolving, add 5 millimoles of molybdenum acetylacetonate, stir to form black powder, continue to heat and stir for 2 hours, filter with suction, wash with ethanol, and dry in vacuum at 40°C to obtain a black powder product. Its structural formula is as follows, and its infrared analysis spectru...

Embodiment 2

[0022] Weigh 10 mmol of isoniazid, put it into a round-bottomed flask (50 ml) containing 20 ml of pyridine, heat and stir at 50°C, add 10 mmol of 2-acetylpyridine after the isoniazid is completely dissolved, and stir for 1 After 7 days, the white needle-like crystals were separated by suction filtration and washed with a small amount of ethanol to obtain 2-acetylpyridine isonicotinoid hydrazide Schiff base complex.

[0023] Weigh 5mmol of 2-acetylpyridine-isonicotinic acid hydrazide Schiff base complex, put it into a round-bottomed flask (50ml) containing 15ml of pyridine, heat and stir at 75°C, and wait until 2-acetyl-pyridine-isonicotinic acid hydrazide is completely dissolved Finally, add 5 millimoles of molybdenum acetylacetonate, stir to have black powder precipitate out, continue to heat and stir for 2 hours, then suction filter, wash with pyridine, and dry in vacuum at 40°C to obtain the product. Its structural formula is as follows, and its infrared analysis spectrum an...

Embodiment 3

[0026] Take tert-butyl hydroperoxide, n-propanol and 2-acetylpyridine isonicotinoid hydrazide molybdenum complex synthesized in [Example 1] and put them into a high-pressure reactor, seal the reactor and start heating and stirring. When the preset 100°C is reached, the high-pressure pump pumps in propylene, and the amount of propylene is determined by the pumped volume. Reaction timing, after reaching 2 hours, take off the reaction kettle, cool to 10-15°C with ice water, and take the liquid phase into a frozen sampler. Continue to freeze the sampler at minus 20°C for 30 minutes, then unscrew the air valve, slowly release the propylene in the sampler, open the sampler, quickly transfer the remaining liquid to the chromatographic sampling bottle, seal it, and perform chromatographic analysis.

[0027] Reaction conditions: reaction temperature 100°C, reaction time 2 hours, rotating speed 540rpm, tert-butyl hydroperoxide (TBHP) addition 70 millimoles, n-propanol addition 50 millim...

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Abstract

The invention relates to a 2-acetylpyridine o-aminophenol molybdenum complex and a preparation method thereof, mainly solving the problem that a molybdenum Schiff alkali coordination compound is undisclosed in previous patents. The technical scheme of the invention is adopted to solve the problem, and in the technical scheme, the chemical structural formula of the 2-acetylpyridine isonicotinyl hydrazide molybdenum complex is shown in the specification, wherein R1 is selected from -OHR2 or R2 is CnH2n+1, and n is 2-10. The preparation method can be applied to the industrial production of the 2-acetylpyridine isonicotinyl hydrazide molybdenum complex.

Description

technical field [0001] The invention relates to a 2-acetylpyridine isoniazid molybdenum complex and a preparation method thereof. Background technique [0002] Schiff base refers to a class of organic compounds containing imine or azimine characteristic groups (-RC=N-), which are formed by condensation of carbonyl and amino groups of aldehydes and ketones under certain conditions. Due to the hyperconjugation between the C=N bond and the benzene ring, such compounds are generally relatively stable. The benzene ring contains Schiff bases with coordination functional groups such as -OH and -N. The intramolecular hydrogen bonding makes it have a rigid structure, and it is very easy to form complexes with high-valent metals as multi-dentate ligands. Therefore, Schiff bases occupy an important position in coordination chemistry. [0003] Schiff bases are an important class of organic synthesis reagents and intermediates. Schiff base compounds and their metal complexes have impo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F11/00B01J31/22C07D303/04C07D301/19
Inventor 王戈宋纪元陶乔杨穆谭丽高焕新金国杰
Owner CHINA PETROLEUM & CHEM CORP
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