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Method for catalytically synthesizing aminated compounds by using carbon-silicon solid acid as catalysts

A solid acid and catalyst technology, applied in the preparation of organic compounds, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of excess reagents, harsh reaction conditions, long reaction time, etc., to achieve short reaction time, mild reaction conditions, The effect of a small amount of catalyst

Inactive Publication Date: 2010-07-21
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most reactions are limited by a large excess of reagents, long reaction times, and harsh reaction conditions.

Method used

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  • Method for catalytically synthesizing aminated compounds by using carbon-silicon solid acid as catalysts
  • Method for catalytically synthesizing aminated compounds by using carbon-silicon solid acid as catalysts
  • Method for catalytically synthesizing aminated compounds by using carbon-silicon solid acid as catalysts

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Conjugate Addition Reaction of Methyl Acrylate and Cyclohexylamine

[0026] The preparation of the first step carbon silicon solid acid

[0027] Add 6g P123, 180g 2M HCl and 45g H to a 500ml beaker 2 O, put it in a 40°C water bath and stir for 4 hours, then add 12.75g TEOS, continue to stir for 24 hours, put it into a reaction kettle with a polytetrafluoroethylene liner, crystallize in a 100°C oven for 24 hours, wash with water, filter with suction, and dry Dry it, and finally burn it in a muffle furnace at 550°C for 6 hours to obtain SBA-15 powder. Take 0.1g of oxalic acid, 15ml of absolute ethanol, 2.67g of furfuryl alcohol and 3.0g of SBA-15 and stir at room temperature for 4h, then put them in an oven at 80°C and an oven at 160°C for 6h each, 2 Burn at 500°C for 6h. Finally, use oleum to sulfonate at 120°C for 48 hours, wash with hot water, filter with suction, and dry to obtain functionalized carbon-silicon solid acid.

[0028] Step 2 Conjugate addition reactio...

Embodiment 2～5

[0033] Except for the following differences, all the other are the same as in Example 1, the amount of catalyst is 0.04g, the amount of methyl acrylate is 0.02mol, the amount of cyclohexylamine is according to the ratio in Table 1, and the reaction is carried out for 10min.

[0034] Table 1

[0035]

Embodiment 6～9

[0037] Except the following difference, all the other are the same as Example 1, methyl acrylate is 0.02mol, cyclohexylamine is 0.028mol, and solid acid catalyst is according to the consumption of Table 2 respectively, reacts 10min.

[0038] Table 2

[0039]

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PUM

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Abstract

The invention discloses a method for catalytically synthesizing aminated compounds by using carbon-silicon solid acid as catalysts. In the method, alpha, beta-unsaturated ester and amine are used as raw materials, the carbon-silicon solid acid is used as the catalysts, the catalysts use furfuryl alcohol as carbon sources and use fuming sulphuric acid as sulfonating reagents, and sulfonic groups are introduced on amorphous carbon generated after the carbonization of the furfuryl alcohol. The conversion rate of reactants of the invention is higher than 97.0 percent, the product selectivity is higher than 97.3 percent, the operation is simple, the reaction time is short, no solvent is needed, the catalysts recovered after the completion of the reaction can be reused, and the activity maintains unchanged.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for synthesizing amine compounds by using functionalized carbon-silicon solid acid as a catalyst to catalyze the conjugated addition of α, β-unsaturated esters and amines. Background technique [0002] Acid catalysts are indispensable in the modern chemical industry, and are widely used in the manufacture of various products such as pharmaceuticals, petrochemical products, and polymer products. Solid acid has the advantages of good activity, long service life, simple post-treatment, and easy reuse, especially the catalytic reaction using solid acid has been widely used in petrochemical and petroleum refining production processes [Min Enze et al., Chemical Bulletin, 1999, 3(5): 10-15]. The research on solid acid has also become one of the hotspots in current catalytic research. Solid acid catalysts can be used in a variety of acid-catalyzed reactions,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/08C07C229/14C07C229/24C07C229/12B01J29/03
Inventor 杨建国陈露朱娟鲍少华纪永军张硕苏秦
Owner EAST CHINA NORMAL UNIV
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