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Transition metal catalyst and method for preparing picoline through adopting catalyst

A transition metal and catalyst technology, applied in the field of preparing methyl pyridine, can solve the problems of high reaction temperature, low yield, difficult product separation, etc., and achieve the effects of good production safety and high catalytic efficiency

Active Publication Date: 2013-04-10
北京颖泰嘉和分析技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method for producing 2-picoline mainly contains two kinds, one is to refine 2-picoline with coal tar, the main defect of this method is low yield, poor quality, and coal tar resources are also quite poor; the other The first is to produce 2-picoline by the ammonia aldehyde method. The reaction temperature of this method is as high as 550 ° C, and the product contains pyridine, 3-picoline, 4-picoline, 2-methyl-5-ethylpyridine, The boiling points of these by-products are too close, and the separation of the products is difficult, thus affecting the quality of 2-picoline

Method used

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  • Transition metal catalyst and method for preparing picoline through adopting catalyst
  • Transition metal catalyst and method for preparing picoline through adopting catalyst
  • Transition metal catalyst and method for preparing picoline through adopting catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] This example is used to illustrate the transition metal catalyst provided by the present invention.

[0019] At room temperature, in a nitrogen atmosphere, mix 2 moles of sodium tetramethylcyclopentadienyl and 1.2 moles of anhydrous CoCl 2 Add 300 ml of tetrahydrofuran for contact reaction for 2 hours, vacuum filter the mixture obtained after the reaction (absolute pressure is 0.01MPa), and then crystallize by evaporation to obtain purple-black crystals, which are analyzed by nuclear magnetic resonance and mass spectrometry. It is known that the crystal is the transition metal catalyst A1 shown in structural formula 1,

[0020] Structural formula 1

[0021]

Embodiment 2

[0023] This example is used to illustrate the transition metal catalyst provided by the present invention.

[0024] At room temperature, in a nitrogen atmosphere, mix 2 moles of indenyl sodium and 1.2 moles of anhydrous CoCl 2 Add 200 ml of tetrahydrofuran for contact reaction for 2.5 hours, vacuum filter the mixture obtained after the reaction (absolute pressure, that is, the vacuum degree is 0.01MPa), and then crystallize by evaporation to obtain purple-black crystals, and analyze by nuclear magnetic resonance and mass spectrometry. Knowing that the crystal is the transition metal catalyst A2 shown in structural formula 2,

[0025] Structural formula 2

[0026]

Embodiment 3

[0028] This example is used to illustrate the transition metal catalyst provided by the present invention.

[0029] At room temperature, in a nitrogen atmosphere, mix 2 moles of sodium fluorenyl and 1.3 moles of anhydrous CoCl 2 Add 400 ml of tetrahydrofuran for contact reaction for 2.5 hours, vacuum filter the mixture obtained after the reaction (absolute pressure, that is, the vacuum degree is 0.01MPa), and then crystallize by evaporation to obtain purple-black crystals, analyzed by nuclear magnetic resonance and mass spectrometry It is known that the crystal is the transition metal catalyst A3 represented by structural formula 3.

[0030] Structural formula 3

[0031]

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PUM

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Abstract

The invention provides a transition metal catalyst, wherein the structural general formula of the catalyst is R1(Z)yMR2, wherein R1 and R2 are same or different, and are respectively substituted or unsubstituted cyclopentadienyl, substituted or unsubstituted indenyl and substituted or unsubstituted fluorenyl, wherein y is 0 or 1, Z is a linked group for connecting R1 and R2, and M is transition metal element. The invention further provides a method for preparing picoline, wherein the method comprises leading acetylene and methyl cyanide to contact for reacting under the existence of catalyst,and the catalyst is the transition metal catalyst supplied by the invention. The transition metal catalyst can effectively prompt methyl cyanide and acetylene to react for preparing 2-picoline.

Description

Technical field [0001] The invention relates to a transition metal catalyst and a method for preparing picoline by using the transition metal catalyst. Background technique [0002] Picoline is an important chemical intermediate and an important raw material for fine chemicals. It can be used in many fields, for example, as a raw material for medicine and agrochemicals. In the picoline series, 2-picoline can be used to produce long-acting guanamine, anti-allergic drug chlorpheniramine, pesticide intermediates, feed and feed intermediates, and can also be used to prepare herbicide drugs. At present, there are two main methods for producing 2-methylpyridine. One is to extract 2-methylpyridine from coal tar. The main disadvantages of this method are low yield and poor quality, and coal tar resources are also quite scarce; One is to use the aminoaldehyde method to produce 2-methylpyridine. The reaction temperature of this method is as high as 550℃, and the product contains pyridine,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07D213/16C07D213/12
Inventor 王开杨瑜杰王龙王大文
Owner 北京颖泰嘉和分析技术有限公司
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