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Preparation method of floralozone

A sea breeze aldehyde and isobutyraldehyde technology, applied in the field of preparation of organic compounds, can solve the problems of high cost of raw materials, increased unsafe factors, unfavorable solvent recycling, etc.

Active Publication Date: 2014-08-06
SUQIAN COSMOS CHEM
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0007] 3. Improper post-treatment method, the acidic or alkaline system after treatment will make the product easy to decompose in the later stage of rectification
[0012] 3. The reaction system is more complex, which is not conducive to the recovery and utilization of solvents;
[0013] 4. The system uses tetrahydrofuran, which increases unsafe factors
[0014] In addition, in this document, hydrobromic acid and acetic acid are used as bromomethylation reagents to carry out the electrophilic substitution reaction of aromatic hydrocarbons to prepare ethyl benzyl bromide. Bromine, the process is cumbersome, and the "three wastes" are produced in a large amount
[0015] From the technical analysis of existing patents and documents, it can be seen that there are many problems in the existing process for preparing sea breeze aldehyde, such as high catalyst and post-treatment costs, catalysts that cannot be recovered or recycled, and intermediates required for the preparation of sea breeze aldehyde The yield of ethyl benzyl halide is low, and the whole reaction produces more waste water, which is not conducive to environmental protection

Method used

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Examples

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preparation example Construction

[0023] According to the present invention, a kind of method for preparing sea breeze aldehyde is provided, and this preparation method comprises following 3 steps:

[0024] Step 1, add ethyl benzyl chloride, sodium hydroxide, water, quaternary ammonium salt phase transfer catalyst and ethylbenzene in the reaction kettle, mix and stir evenly, wherein, the consumption of said ethyl benzyl chloride is ethyl benzyl chloride 0.2 to 10 times the weight, the molar ratio of sodium hydroxide to ethyl benzyl chloride is 1 to 10:1, and the amount of the quaternary ammonium phase transfer catalyst is 0.2 to 20 wt% of ethyl benzyl chloride .

[0025] According to the present invention, strong base sodium hydroxide is used to attack the α-H of isobutyraldehyde, and the isobutyraldehyde that loses a proton generates a carbanion with strong nucleophilicity, which undergoes a nucleophilic substitution reaction with ethyl benzyl chloride.

[0026] The amount of sodium hydroxide is such that th...

Embodiment 1

[0069] With 400g of ethyl benzyl chloride, wherein the contents of 2-ethyl / 4-ethyl / 3-ethyl benzyl chloride are respectively 25%, 69%, and 2%, 199.5g of sodium hydroxide, 112.2g of water, Add 8g tetrabutylammonium bromide and 200g ethylbenzene into the reaction kettle, mix and stir evenly;

[0070] Then the reaction kettle was heated to 50°C, and 197.7g of isobutyraldehyde was added dropwise under the condition of controlling the reaction temperature, and after the dropwise addition was completed, it was kept at 70°C for 10 hours;

[0071] Cool the reaction kettle to 10°C, filter the reaction system, and separate the liquid at room temperature. The water phase after liquid separation is recycled. The organic phase is washed with acetic acid solution and water, and the solvent is removed from the washed organic phase. Pressure rectification, obtains the fraction of target product sea breeze aldehyde, and its yield is 77%.

[0072] Detected by gas chromatography, the content of ...

Embodiment 2

[0074] With 400g of ethyl benzyl chloride, wherein the contents of 2-ethyl / 4-ethyl / 3-ethyl benzyl chloride are respectively 25%, 69%, and 2%, 199.5g of sodium hydroxide, 112.2g of water, Add 8g tetrabutylammonium chloride and 200g ethylbenzene into the reaction kettle, mix and stir evenly;

[0075] Then the reaction kettle was heated to 130°C, and 197.7g of isobutyraldehyde was added dropwise under the condition of controlling the reaction temperature, and after the dropwise addition was completed, it was kept at 80°C for 15 hours;

[0076] Cool the reaction kettle to 15°C, filter the reaction system and separate the liquid at room temperature, recycle the water phase after liquid separation, add acetic acid solution and water to the organic phase, remove the solvent from the washed organic phase, and carry out dehydration Pressure rectification, obtains the cut of target product sea breeze aldehyde, and its yield is 81%.

[0077] Detected by gas chromatography, the content o...

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Abstract

The invention discloses a preparation method of floralozone. The preparation method comprises the steps of dropwise adding isobutyraldehyde into an ethyl benzyl chloride contained reaction system through controlling the reaction temperature under the action that sodium hydroxide and quaternary ammonium salt compounds are used as phase transfer catalysts, and finally, preparing at the yield of 70-85% to obtain floralozone with the content up to more than 94%. The preparation method of floralozone, disclosed by the invention, is low in yield of three wastes, strong in process operability and low in cost.

Description

technical field [0001] The invention relates to a preparation method of organic compounds, in particular to a preparation method of sea breeze aldehyde. Background technique [0002] The compound that replaces phenylpropanal series has the fragrance of lily of the valley and rabbit ear grass, and the fresh air style. It is called sea breeze aldehyde. Its fragrance is elegant and long-lasting. value. [0003] In the prior art, sea breeze aldehyde is mostly synthesized by using ethyl benzyl halide as the starting material, which is obtained by condensation with isobutyraldehyde under the action of a catalyst. [0004] In "Chemical World" 09, 1988, "Phase Transfer Catalytic Synthesis of Sea Breeze Aldehyde", under the action of a phase transfer catalyst, ethyl benzyl chloride and isobutyraldehyde were mixed and dropped, and under the action of sodium hydroxide, the synthesis Sea Breeze Aldehyde. This method has the following drawbacks: [0005] 1. Those with better reaction...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/68C07C47/228
CPCC07C17/32C07C45/68C07C47/228C07C22/04
Inventor 王宁宁陈思黄进刘建生葛建军唐梁平
Owner SUQIAN COSMOS CHEM
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