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2-Acetylpyridine adenoaminophenol molybdenum complex and preparation method thereof

A technology of acetylpyridine and o-aminophenol, which is applied in the field of 2-acetylpyridine condensed o-aminophenol molybdenum complex and its preparation field, can solve problems such as no molybdenum Schiff base complex, and achieve excellent catalytic performance, Good stability and simple operation

Active Publication Date: 2016-05-18
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 adenoaminophenol molybdenum complex and preparation method thereof
  • 2-Acetylpyridine adenoaminophenol molybdenum complex and preparation method thereof
  • 2-Acetylpyridine adenoaminophenol molybdenum complex and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Weigh 10 millimoles of o-aminophenol, put it into a round-bottomed flask (50 milliliters) containing 20 milliliters of absolute ethanol, heat and stir at 50° C., add 10 millimoles of 2-acetylpyridine after the o-aminophenol is completely dissolved, and stir for 1 After standing for one hour, light yellow polyhedral crystals were precipitated after 6 days. Filtrate with suction and wash with a small amount of ethanol to obtain 2-acetylpyridine o-aminophenol Schiff base.

[0019] Weigh 5mmol of 2-acetylpyridine-o-aminophenol, put it into a round-bottomed flask (50ml) containing 15ml of absolute ethanol, heat and stir at 75°C, and add 5mmol of acetylacetone after the 2-acetylpyridine-o-aminophenol is completely dissolved Molybdenum, stirred brown powder to precipitate, continue to heat and stir for 2 hours, then cool and suction filter, wash with ethanol and dry in vacuum at 40°C to obtain a brown powder product, its structural formula is as follows, and its infrared analy...

Embodiment 2

[0022] Weigh 10 mmol of o-aminophenol, 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 o-aminophenol is completely dissolved, and stir for 1 hour After standing still, light yellow polyhedral crystals were precipitated after 6 days. Filtrate with suction and wash with a small amount of ethanol to obtain 2-acetylpyridine o-aminophenol Schiff base.

[0023] Weigh 5mmol of 2-acetylpyridine-o-aminophenol, put it into a round-bottomed flask (50ml) containing 15ml of pyridine, heat and stir at 75°C, and add 5mmol of molybdenum acetylacetonate after the 2-acetylpyridine-o-aminophenol is completely dissolved. Stir brown powder to precipitate, continue to heat and stir for 2 hours, then cool and 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 is consistent with figure 1 resemblance.

[00...

Embodiment 3

[0026] Take tert-butyl hydroperoxide, n-propanol and the 2-acetylpyridine adenoaminophenol 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 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.

[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 millimoles, catal...

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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 o-aminophenol 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 o-aminophenol molybdenum complex.

Description

technical field [0001] The invention relates to a molybdenum complex compound of 2-acetylpyridine condensed o-aminophenate 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 thei...

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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