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Method for preparing ketal in ionic liquid

A technology of ionic liquids and acidic ionic liquids, applied in the formation/introduction of ether groups/acetal groups/ketal groups, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problem of using volatile organic solvents and toxic catalysts Harmful, non-recyclable and other problems, to achieve high selectivity, convenient operation, and simplified separation process

Inactive Publication Date: 2006-11-08
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a green method for preparing ketals, which solves the defects in the prior art, such as poisonous and harmful catalysts, corrosion of equipment and failure to recycle, use of volatile organic solvents, and production of a large amount of industrial waste, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0020] Add 0.5 mole of acetone and 1 mole of ethanol mixed solution to 1 mole of [Et 3 NH][HSO 4 ] In the acidic ionic liquid, add 60 grams of 4A molecular sieves and stir for 1.5 hours. Filtration, solid-liquid separation, solution phase static layering. Since the product ketal is insoluble in [Et 3 NH][HSO 4 ] acidic ionic liquid, while acetone and ethanol can be dissolved in [Et 3 NH][HSO 4 ] In the acidic ionic liquid. The product is directly obtained by phase separation and pouring, with a product yield of 90% and a content of 97%. The unreacted raw materials were evaporated from the acidic ionic liquid under heating conditions and used mechanically. The used 4A molecular sieve can continue to be used for the next reaction after being heated and dehydrated in the ionic liquid.

Embodiment example 2

[0022] Add 0.5 mol of acetone and 1 mol of methanol mixed solution to 2 mol of [Et 3 NH][HSO 4 ] In the acidic ionic liquid, 1 mole of calcium sulfate was added subsequently, and the reaction was stirred for 1.5 hours. After the reaction is finished, filter, separate the solid from the liquid, and separate the calcium sulfate, and the solution phase is allowed to stand for stratification. Since the product ketal is insoluble in [Et 3 NH][HSO 4 ] acidic ionic liquid, while acetone and methanol can be dissolved in [Et 3 NH][HSO 4 ] In the acidic ionic liquid. The product is directly obtained by phase separation and pouring, with a product yield of 88% and a content of 97%. The unreacted raw materials were evaporated from the acidic ionic liquid under heating conditions and used mechanically. The calcium sulfate used subsequently can continue to be used as the next reaction after being heated and dehydrated in the ionic liquid.

Embodiment example 3

[0024] Add 0.5 mole of butanone and 1 mole of methanol mixed solution to 2 moles of [Bmim][HSO 4 ] In the acidic ionic liquid, 1 mole of calcium sulfate was added subsequently, and the reaction was stirred for 1 hour. After the reaction is finished, the calcium sulfate is separated by filtration, and the solution phase is allowed to stand for stratification. Since the product ketal is insoluble in [Bmim][HSO 4 ] in acidic ionic liquids, while methyl ethyl ketone and methanol can be dissolved in [Bmim][HSO 4 ] In the acidic ionic liquid. The product is directly obtained by phase separation, with a product yield of 80% and a content of 97%. The unreacted raw materials were evaporated from the acidic ionic liquid under heating conditions and used mechanically. The calcium sulfate used subsequently can continue to be used as the next reaction after being heated and dehydrated in the ionic liquid.

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PUM

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Abstract

The present invention relates to new method of preparing ketal. Alcohol and ketone as initial materials produce condensation reaction in acid ionic liquid as catalyst and reaction solvent and in the presence of water absorber to synthesize ketal in high selectivity and high yield. The method is one kind of green synthesis method without using volatile organic solvent and additional catalyst.

Description

technical field [0001] The present invention relates to a new method for preparing ketal. In particular, it relates to a method for synthesizing ketal by condensation reaction with alcohol and ketone as starting raw materials, acidic ionic liquid as catalyst and reaction solvent. Background technique [0002] Ketal is an important form of protecting carbonyl groups, and it is also a large class of important fine chemical intermediates. For example, 2,2-dimethoxypropane, 2,2-diethoxypropane is a synthetic perfume and pharmaceutical intermediate 2-methoxypropene, 2-ethoxypropene, linalool, nerolidol, Farnesyl acetone, isophytol, key intermediates of ionone, vitamin A, β-carotene, etc.; cyclohexanone diisopropanol is an important intermediate for the synthesis of broad-spectrum antibiotic clarithromycin. Ketals are widely used in the fragrance and pharmaceutical industries. [0003] Because ketals have important applications in the fields of fine chemicals, pharmaceutical in...

Claims

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Application Information

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IPC IPC(8): C07D317/72B01J31/02C07B41/04C07C41/56C07C43/303C07C43/305
Inventor 李浩然姜辉王从敏崔伟
Owner ZHEJIANG UNIV
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