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Method for preparing acetal compound by room-temperature ionic liquid catalyst

A room temperature ionic liquid, catalytic preparation technology, used in the preparation of organic compounds, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc. To achieve the effect of reducing pollution, simple preparation and mild reaction conditions

Inactive Publication Date: 2009-09-30
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the defects in the prior art that the catalyst is poisonous and harmful, corrodes equipment and cannot be recycled, uses volatile organic solvents and produces a large amount of industrial waste, and provides a highly efficient and reusable catalyst. Method for preparing acetal compounds under environmentally friendly and mild reaction conditions

Method used

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  • Method for preparing acetal compound by room-temperature ionic liquid catalyst
  • Method for preparing acetal compound by room-temperature ionic liquid catalyst
  • Method for preparing acetal compound by room-temperature ionic liquid catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0036] In the 100mL round bottom flask, add 11.8g of 37% aqueous formaldehyde solution successively, methyl alcohol 9.3g and N-methyl-N'-butanesulfonate methyl imidazole methyl sulfate ionic liquid 1g (catalyst, formaldehyde and methanol mol ratio are 0.02 : 1: 2), after heating at 75° C. for 2 hours and fully refluxing, the methylal content in the reaction solution was 38% and the selectivity was 92% according to chromatographic analysis.

Embodiment 2

[0038] In the 100mL round bottom flask, add 50% formaldehyde aqueous solution 8.5g successively, methyl alcohol 9.3g and N-methyl-N'-butanesulfonate methyl imidazole methyl sulfate ionic liquid 1g (catalyst, formaldehyde and methanol mol ratio are 0.02 : 1: 2), after heating at 75° C. for 2 hours, the methylal content in the reaction solution was 52% and the selectivity was 84% ​​according to chromatographic analysis.

Embodiment 3

[0040] In the 100mL round bottom flask, add 11.8g of 37% aqueous formaldehyde solution successively, methanol 18.6g and N-methyl-N'-butanesulfonate methylimidazole methyl sulfate ionic liquid 1g (catalyst, formaldehyde and methanol mol ratio are 0.02 : 1: 4), after heating at 75° C. for 2 hours and fully refluxing, the methylal content in the reaction solution was 56% and the selectivity was 97% according to chromatographic analysis.

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Abstract

The invention discloses a method for synthesizing an acetal compound by taking a room-temperature ionic liquid as a catalyst. The method comprises the following step: taking aldehyde or aldehyde-ethanol as a reactant, and synthesizing the acetal compound in the presence of no other organic solvent and dehydrating agent. Compared with the prior synthesizing method, the method has mild reaction conditions, does not use strongly corrosive acid, such as sulfuric acid, hydrochloric acid, and the like as catalyst, and does not use other organic solvent and dehydrating agent any longer. The method has the characteristics of simple operation, high catalytic activity, good selectivity, reusage, and the like. Thus, the method has good application prospect.

Description

technical field [0001] The invention relates to a method for synthesizing acetal compounds by using room temperature ionic liquid as a catalyst. Background technique [0002] Carbonylation reaction is an important class of organic reaction, which has a wide range of applications in organic synthesis, industrial production and other fields. Acetal compounds are stable in nature, and most of them have special aroma. They are high-end new spices developed in the past ten years. In organic synthesis, acetal (ketone) is often used to protect the carbonyl group. In addition, acetal (ketone) compounds are also commonly used as intermediates and target products in the synthesis of steroids and sugars, paint and pharmaceutical industries, and even Can be used as a special reaction solvent. For example, methylal can be used to prepare anion exchange resin, oxidize to produce high-concentration formaldehyde and polyacetal resin, etc.; acetal is an important wine additive, and is also...

Claims

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Application Information

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IPC IPC(8): C07D323/06C07C41/56C07C43/303B01J31/02
Inventor 夏春谷李臻沈志强陈静刘佳梅唐中华
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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