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Method for preparing unsaturated ketone

An unsaturated and modified technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of carbon-based compounds, etc., can solve problems such as low yield

Active Publication Date: 2019-03-22
SHANDONG NHU VITAMIN CO LTD +1
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  • Abstract
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  • Application Information

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Problems solved by technology

[0005] The invention provides a method for preparing unsaturated ketones. On the one hand, the preparation method improves the yield of the reaction, solves the problem of low yields catalyzed by conventional acidic resins, and on the other hand does not leave acid residues in unsaturated ketone products. , avoiding the impact on the subsequent hydrogenation quality of unsaturated ketones

Method used

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  • Method for preparing unsaturated ketone
  • Method for preparing unsaturated ketone
  • Method for preparing unsaturated ketone

Examples

Experimental program
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Effect test

Embodiment 1

[0036] according to figure 1 The reaction flow diagram shown in the reaction is carried out, and the feed flow of tertiary nerolidol and 2-methoxypropene is regulated by a metering pump, and the feed flow of tertiary nerolidol is: 0.088ml / s, 2-methoxy The feeding flow rate of base propylene is: 0.1ml / s, the filling volume of acidic resin in the fixed bed is 2.0L, and the molar ratio of dehydronerolidol and 2-methoxypropylene is 1:4. After fully mixing through the mixer, use Preheat it to 100°C by means of external heating, and enter the acid resin bed from the top. The acid resin is a macroporous acid resin modified by tributylmethylammonium chloride. The bed temperature is 120°C, and the residence time is 3h. After passing through the condenser, it enters the material storage tank. The discharge pipe is equipped with a sampling port, which can monitor the reaction in the fixed bed at any time. The apparent content of the reaction product is 93%, and the yield is 89%.

[0037...

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Abstract

The invention discloses a method for preparing unsaturated ketone. According to the method, an unsaturated alcohol and 2-alkoxy propylene are adopted as raw materials, an acid resin in a fixed bed aremodified, a Saucy-Marbet reaction is carried out, and unsaturated ketone is synthesized with high selectivity and high yields. According to the method, the modified acid resin is adopted as a catalyst, the problem that a common acid resin is poor in catalysis effect is solved; in addition, a fixed bed reactor is adopted to catalyze reactions, separation of the catalyst from reaction products before and after reactions can be achieved, equipment corrosion and adverse influence of a great amount of acids upon later industrial aftertreatment can be avoided, and the method is an economic and efficient synthesis method.

Description

technical field [0001] The invention belongs to the technical field of acid-catalyzed preparation of unsaturated ketones, and in particular relates to a method for preparing unsaturated ketones by Saucy-Marbet reaction in a fixed-bed reactor using a modified immobilized acid as a catalyst. Background technique [0002] Unsaturated ketones are important starting materials for the synthesis of flavors and fragrances and pharmaceutical intermediates, such as methyl heptenone, pseudoionone, etc., due to the prominent position of this unsaturated ketone in the chemical industry, many scholars have made their synthetic methods A lot of research has been done. US6184420 provides a reaction method for synthesizing unsaturated ketones from propargyl alcohol and ethers under acid catalysis; CN98120681 provides a method for synthesizing γ, δ- A method for monounsaturated / or β, γ, δ-diunsaturated ketones; CN200980142015.9 provides a method for tertiary vinyl carbinol and isopropenyl me...

Claims

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Application Information

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IPC IPC(8): C07C45/51C07C49/203C07C45/62C07C49/04B01J31/08
CPCC07C45/513C07C45/62B01J31/08C07C49/203C07C49/04
Inventor 黄高峰赵贺赵德胜严宏岳
Owner SHANDONG NHU VITAMIN CO LTD
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