Carbon-nitrogen material loaded cobalt catalyst and method for synthesizing pimavanserin intermediate

A technology of cobalt catalyst and carbon-nitrogen material, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of poor chemical stability, unfavorable industrial applications, hidden safety hazards, etc., and achieve convenient synthesis process and reduce Synthesis cost, life extension effect

Active Publication Date: 2016-12-07
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Sodium triacetoxyborohydride has high hygroscopicity in the air, poor chemical stability and high price. Large-scale production has certain safety hazards, which is not conducive to industrial application.

Method used

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  • Carbon-nitrogen material loaded cobalt catalyst and method for synthesizing pimavanserin intermediate
  • Carbon-nitrogen material loaded cobalt catalyst and method for synthesizing pimavanserin intermediate
  • Carbon-nitrogen material loaded cobalt catalyst and method for synthesizing pimavanserin intermediate

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0019] The synthesis of embodiment 1 catalyst A

[0020] Weigh 0.249g of cobalt acetate tetrahydrate in a round bottom flask, 30ml of methanol as a solvent, then add 0.472g of IL1 (the molar ratio of metal cobalt compound to IL1 is 1:3), stir at room temperature for 30min, then slowly add 1.0g of activated carbon (Based on a Co loading of 6% by mass). Put the round-bottomed flask into an oil bath at 50° C. and heat and stir for 5 h, then remove the solvent methanol by rotary evaporation. The obtained supported pre-catalyst was vacuum-dried at 60° C. for 12 hours. The dried pre-catalyst was placed in a tube furnace and calcined at 800°C for 2h under nitrogen (heating rate 5°C / min). After naturally lowering to constant temperature, catalyst A was obtained.

Example Embodiment

[0021] The synthesis of embodiment 2 catalyst B

[0022] Weigh 0.249g of cobalt acetate tetrahydrate in a round bottom flask, 30ml of methanol as a solvent, then add 0.547g of IL2 (the molar ratio of metal cobalt compound to IL2 is 1:3), stir at room temperature for 30min, then slowly add 1.0g of activated carbon (Based on a Co loading of 6% by mass). Put the round-bottomed flask in an oil bath at 55° C. and heat and stir for 5 h, then remove the solvent methanol by rotary evaporation. The obtained supported pre-catalyst was vacuum-dried at 60° C. for 12 hours. The dried pre-catalyst was placed in a tube furnace and calcined at 800°C for 2h under nitrogen (heating rate 5°C / min). After naturally lowering to a constant temperature, catalyst B was obtained.

Example Embodiment

[0023] The synthesis of embodiment 3 catalyst C

[0024] Weigh 0.249g of cobalt acetate tetrahydrate in a round bottom flask, 30ml of methanol as a solvent, then add 0.508g of IL3 (the molar ratio of metal cobalt compound to IL3 is 1:3), stir at room temperature for 30min, then slowly add 1.0g of activated carbon (Based on a Co loading of 6% by mass). Put the round-bottomed flask into an oil bath at 50° C. and heat and stir for 6 h, then remove the solvent methanol by rotary evaporation. The obtained supported pre-catalyst was vacuum-dried at 60° C. for 12 hours. The dried pre-catalyst was placed in a tube furnace and calcined at 800°C for 2h under nitrogen (heating rate 5°C / min). After naturally lowering to a constant temperature, catalyst C was obtained.

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Abstract

The invention relates to a carbon-nitrogen material loaded cobalt catalyst and a method for synthesizing pimavanserin intermediate. The catalyst is prepared by the following steps: coordinating a metal cobalt compound and cyano-containing ionic liquid in an organic solvent, and impregnating to an activated carbon carrier; and calcining at a specific temperature under an inert gas to obtain a corresponding carbon-nitrogen loaded catalyst. According to the method for catalytically synthesizing pimavanserin intermediate 4-(4-fluorobenzylamino)-1-methylpiperidine by utilizing the catalyst, 4-(4-fluorobenzylamino)-1-methylpiperidine is prepared by reductively aminating 4-flunamine serving as a raw material with N-methyl-4-piperidone or 1-methyl-4-piperidylamine with hydrogen serving as a reducing agent at a certain pressure and temperature. The catalyst has the advantages of low cost, simple preparation method, good stability, high activity and high selectivity, and can be recycled for multiple times, and is suitable for industrial production.

Description

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Claims

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Application Information

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Owner NANJING UNIV OF TECH
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