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Acetylacetone acetal hydrazide molybdenum complex and preparation method thereof

A technology of acetone benzoyl hydrazide molybdenum and acetone benzoyl hydrazide, which is applied in the field of acetylacetonate benzoyl hydrazide molybdenum complex and its preparation field, can solve the problems such as no molybdenum Schiff base complex, etc. Achieve excellent catalytic performance, mild reaction conditions, and simple operation

Active Publication Date: 2015-10-21
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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  • Acetylacetone acetal hydrazide molybdenum complex and preparation method thereof
  • Acetylacetone acetal hydrazide molybdenum complex and preparation method thereof
  • Acetylacetone acetal hydrazide molybdenum complex and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take by weighing 10 mmoles of benzohydrazine, put into a round-bottomed flask (50 milliliters) containing 20 milliliters of absolute ethanol, heat and stir at 75° C., add 12 mmoles of acetylacetone after the benzohydrazide is completely dissolved, and stir for 2 Add 10 millimoles of molybdenum acetylacetonate after 1 hour, gray powder is precipitated, continue to heat and stir for 2 hours, then suction filter, wash with ethanol and dry in vacuum at 40°C to obtain a gray powder product. Its structural formula is as follows, and its infrared analysis spectrum is shown in figure 1 .

[0019]

Embodiment 2

[0021] Weigh 10 mmoles of benzohydrazide, put it into a round-bottomed flask (50 ml) containing 20 ml of pyridine, heat and stir at 75°C, add 12 mmoles of acetylacetone after the benzohydrazide is completely dissolved, and stir for 2 hours Add 10 millimoles of molybdenum acetylacetonate, gray powder is precipitated, continue to heat and stir for 2 hours, filter with suction, wash with pyridine, and dry in vacuum at 40°C to obtain a gray powder product. Its structural formula is as follows, and its infrared analysis spectrum and figure 1 resemblance.

[0022]

Embodiment 3

[0024] Put tert-butyl hydroperoxide, n-propanol and the acetylacetonate benzoyl hydrazide molybdenum complex synthesized in [Example 1] into an autoclave, seal the autoclave 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 reactor, 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.

[0025] Reaction conditions: reaction temperature 100°C, reaction time 2 hours, rotating speed 540rpm, tert-butyl hydroperoxide (TBHP) addition 70 millimoles, n-propanol addition 50 millimoles, catalyst addition 0.1 millim...

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PUM

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Abstract

The invention relates to an acetylacetone shrinkage benzoyl hydrazine molybdenum complex and a preparation method thereof, mainly solving the problem that the former patents do not disclose molybdenum Schiff alkali coordination compounds. The chemical structure formula of the acetylacetone shrinkage benzoyl hydrazine molybdenum complex is shown in the specification, wherein in the formula, R1 is selected from -OHR2 or R2 is CnH2n+1, and n=2-10. The preparation method disclosed by the invention can be used for the industrial production of the acetylacetone shrinkage benzoyl hydrazine molybdenum complex.

Description

technical field [0001] The invention relates to an acetylacetonate benzoyl hydrazide 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 h...

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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