Method for preparing magnetic double-carbene palladium ligand catalyst and using method thereof

A catalyst and magnetic technology, applied in the field of preparation of magnetic double carbene palladium ligand catalyst, can solve the problem of easy deactivation of Suzuki reaction catalyst, and achieve the effect of good yield

Inactive Publication Date: 2013-02-06
INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The present invention will solve the technical problem that the existing Suzuki reaction catalyst is easily deactivated; and provide a preparation method and a method of use of the magnetic biscarbene palladium ligand catalyst

Method used

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  • Method for preparing magnetic double-carbene palladium ligand catalyst and using method thereof
  • Method for preparing magnetic double-carbene palladium ligand catalyst and using method thereof
  • Method for preparing magnetic double-carbene palladium ligand catalyst and using method thereof

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specific Embodiment approach 1

[0013] Specific embodiment one: the preparation method of magnetic double carbene (NHC) palladium ligand catalyst in the present embodiment is carried out according to the following steps:

[0014] 1. Add 8.24g of strong base into 40mL of organic solvent to obtain suspension A, then add the imidazole solution with a concentration of 2.5g / mL dropwise while stirring at 10-12°C, and keep the temperature at 10-12°C during the dropping process. 12°C, the amount of imidazole solution is 20mL, the solvent in the imidazole solution is the same as the organic solvent used to prepare the suspension A, after the dropwise addition, stir at 10-12°C for 1-8h, then add dropwise (15min. ) 0.5-1mol silane coupling agent, heated to reflux at the boiling point of the organic solvent for 10-24h, cooled to room temperature, added 40mL dichloromethane (CH 2 Cl 2 ), filtered, and the solvent was distilled off, and the fraction at 150° C. was collected by distillation under reduced pressure to obtai...

specific Embodiment approach 2

[0018] Embodiment 2: This embodiment differs from Embodiment 1 in that: Step 1 adds the imidazole solution dropwise and takes 20 minutes to 40 minutes. Other steps and parameters are the same as in the first embodiment.

specific Embodiment approach 3

[0019] Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that the strong base in step 1 is sodium hydroxide, potassium hydroxide, sodium hydride or potassium tert-butoxide. Other steps are the same as those in Embodiment 1 or 2.

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Abstract

The invention discloses a method for preparing a magnetic double-carbene palladium ligand catalyst and a using method thereof, and belongs to the field of Suzuki reaction. The method solves the technical problem that the conventional Suzuki reaction catalyst is easily inactivated. The method comprises the following steps of: 1, preparing alkoxy silicified imidazole; 2, preparing alkoxy silicified double-imidazolyl ligand; 3, preparing Fe3O4 supported double-imidazolyl ligand; and 4, preparing the magnetic double-carbene palladium ligand catalyst. Magnetic separation of the catalyst can be realized by supporting the homogeneous palladium ligand catalyst on the surface of super-paramagnetic Fe3O4. The magnetic double-carbene (NHC) palladium ligand catalyst applied to the Suzuki reaction can completely convert bromobenzene with electron donating group or electron attracting group; and after the catalyst is used for 7 times, the catalytic activity does not decline, for the supporting amount of active ingredients does not decline obviously.

Description

technical field [0001] The invention belongs to the field of Suzuki reaction; in particular, it relates to a preparation method and a use method of a magnetic double carbene palladium ligand catalyst. Background technique [0002] Homogeneous catalysis has made significant progress in the Suzuki reaction (Suzuki reaction). Typical homogeneous catalytic systems such as carbene (NHC) and biphenylphosphine (Phos) ligand palladium catalytic systems have high activity and achieved difficult Activation of activated chlorinated aromatics. However, because the accumulation and precipitation of metals will lead to the loss of activity of homogeneous catalysts, this is an urgent problem to be solved in large-scale production. The complexation of homogeneous palladium ligand catalysts is an effective way to solve this problem. Contents of the invention [0003] The invention solves the technical problem that the existing Suzuki reaction catalyst is easily deactivated; and provides ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28
Inventor 白雪峰王亮吕宏飞
Owner INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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