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A kind of synthesis technique of organic synthesis intermediate cyclohexanone ethylene glycol ketal

A cyclohexanone ethylene glycol ketal and organic synthesis technology, applied in organic chemistry, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of severe equipment corrosion, low product purity, and many side reactions, etc. Achieve the effects of easy access, good yield, and reduced side reactions

Active Publication Date: 2019-06-04
深圳深创生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of this method is that the catalyst is cheap and easy to obtain, and the product yield is high, but this method also has many side reactions, low product purity, serious equipment corrosion, and environmental pollution caused by a large amount of acid contained in wastewater.

Method used

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  • A kind of synthesis technique of organic synthesis intermediate cyclohexanone ethylene glycol ketal
  • A kind of synthesis technique of organic synthesis intermediate cyclohexanone ethylene glycol ketal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The preparation of solid acid catalyst is as follows:

[0022] Step 1. First, 10g of Al2O3 is ultrasonically treated at 120°C for 3 hours in a nitrogen atmosphere;

[0023] Step 2, then mix the treated Al2O3 with 65% H2SO4 solution according to the ratio of solid to liquid mass ratio of 1:12, and reflux and stir for 8 hours;

[0024] Step 3. After reflux and stirring, then stand still for 5 hours, centrifuge, and dry to constant weight at 110°C to obtain Al2O3 as a catalyst active carrier;

[0025] Step 4. Mix the active Al2O3 and 0.5mol / L Fe2(SO4)3 solution at a mass ratio of 1:8, and reflux and stir for 5 hours;

[0026] Step 5, vacuum filtration and separation, the separated solid was mixed with Fe2(SO4)3 solution of the same concentration and volume, and refluxed and stirred for 5 hours under the same conditions, centrifuged and dried at 110°C to constant weight;

[0027] Step 6, using the impregnation method, impregnating the catalyst initially prepared in the pr...

Embodiment 2

[0036] Prepare cyclohexanone, ethylene glycol, and cerium-modified nanoscale composite Fe2(SO4)3 / Al2O3 solid acid catalyst with a mass ratio of 30:32:0.5. Cyclohexanone 30g, ethylene glycol 32g, cerium-modified nano-composite Fe2(SO4)3 / Al2O3 solid acid catalyst 0.5g, water agent cyclohexane 25ml. The operation steps are the same as in Example 1.

Embodiment 3

[0038] Prepare cyclohexanone, ethylene glycol, and cerium-modified nanoscale composite Fe2(SO4)3 / Al2O3 solid acid catalyst with a mass ratio of 40:38:0.5. Cyclohexanone 40g, ethylene glycol 38g, cerium-modified nanoscale composite Fe2(SO4)3 / Al2O3 solid acid catalyst 0.5g. Other raw materials, operation steps are the same with embodiment 1.

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Abstract

The invention discloses a synthesis process of an organic synthetic intermediate cyclohexanone ethylene ketal. The process includes: taking cyclohexanone, ethylene glycol, a water-carrying agent cyclohexane, a self-made cerium modified nanoscale composite Fe2(SO4)3 / Al2O3 solid acid catalyst and the like as the raw materials, and carrying out condensation reflux, vacuum distillation, magnetic stirring and other operations so as to obtain cyclohexanone ethylene ketal.

Description

technical field [0001] The invention relates to a synthesis process of an organic synthesis intermediate cyclohexanone ethylene glycol ketal, belonging to the field of organic synthesis. Background technique [0002] Ketals (aldehydes) are an important class of compounds, which are widely used in wine flavors and daily flavors, and can also be used as intermediates in organic synthesis and carbonyl protection in organic synthesis. Cyclohexanone ethylene glycol ketal is one of these spices. It has floral and mint aromas. It is usually formed by condensation of cyclohexanone and ethylene glycol under the catalysis of inorganic acids such as sulfuric acid, hydrochloric acid, and phosphoric acid. The advantage of this method is that the catalyst is cheap and easy to obtain, and the product yield is high, but this method also has the disadvantages of many side reactions, low product purity, serious corrosion of equipment, and environmental pollution caused by a large amount of ac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/72B01J27/053
CPCB01J27/053C07D317/72
Inventor 庄焕迪柳云萍
Owner 深圳深创生物技术有限公司
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