Production device and method for catalytically synthesizing allyl amyl glycolate perfume with solid acid

Abstract

The invention discloses a production device and method for catalytically synthesizing an allyl amyl glycolate perfume with solid acid. The production method comprises the following steps of by takingdichloroethane as a solvent, under the nitrogen protection condition, performing O-H insertion reaction to obtain isopentyloxy ethyl acetate by adopting a solid rhodium catalyst, ethyl diazoacetate and isoamyl alcohol as starting raw materials, and then performing saponification and acidification to obtain isoamylacetic acid; and then by taking the solid acid as a catalyst, performing condensationreaction on the isoamylacetic acid and allyl alcohol to obtain an allyl amyl glycolate perfume product. By adopting the production device and method, the reaction time is greatly shortened, the process flow is relatively short, the raw materials are available, and the total yield is increased; and for a solid catalyst, solid-liquid separation of the solid acid catalyst is realized by adopting anautomatic backwashing filtration technology, the solid acid catalyst has the advantages of easiness in separation with a liquid phase reaction system, non corrosion to equipment and simpleness in post-treatment, overcomes the problems that existing liquid acid corrodes the equipment, and acid-contained wastewater pollutes environment and is high in selectivity, and solid-liquid separation can be performed at a lower temperature.

Description

technical field [0001] The invention belongs to the technical field of perfume production, and in particular relates to a production device and method for synthesizing glycopyrrolate perfume by solid acid catalysis. Background technique [0002] Gepeng ester, CAS No. 67634-00-8, chemical name allyl isopentoxy acetate, is an important synthetic fragrance, with fruity, delicate fragrance and Gepong and pineapple aroma, widely used in perfumes, cosmetics, soaps , air fresheners, detergents and other products of fragrance. [0003] The traditional production method of glycopyrrolate is as follows: firstly, amyloxyacetic acid is prepared by Williamson reaction, and the yield is about 80%, and then sulfuric acid, perchloric acid, p-toluenesulfonic acid, etc. are used as catalysts to react with allyl alcohol through esterification Obtain Gepong ester; Synthesis of the intermediate amyl amyloxyacetic acid becomes the key to the preparation of allyl amyl amyl amyl acetate. Synthesiz...

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Problems solved by technology

[0003] The traditional production method of glycopyrrolate is as follows: firstly, amyloxyacetic acid is prepared by Williamson reaction, and the yield is about 80%, and then sulfuric acid, perchloric acid, p-toluenesulfonic acid, etc. are used as catalysts to react with allyl alcohol through esterification Obtain Gepong ester; Synthesis of the intermediate amyl amyloxyacetic acid becomes the key to the preparation of allyl amyl amyl amyl acetate. Synthesizing amyl amyl oxyacetic acid first requires the preparation of amyl amyl amyl sodium. At present, there are mainly three kinds of amyl amyl acetate. Method: the one is to use metal sodium as reaction reagent, react dehydrogenation with isoamyl alcohol to prepare sodium isoamyloxide, then use xylene as solvent and chloroacetic acid to react dechlorination sodium to prepare isoamyloxyacetic acid, and the reaction requires anhydrous It is carried out under the system, the process is difficult, the use of sodium metal is dangerous, and it is difficult to realize industrial production; the second is to use sodium hydride as a reaction reagent, and react with isoamyl alcohol in tetrahydrofuran as a solvent to produce sodium alkoxide, and then in dimethyl React with chloroacetic acid in sulfoxide solution to form sodium amyloxyacetate, and then acidify under strong acid conditions to prepare amyloxyacetic acid. The reaction uses sodium hydride, which has extremely strict requirements on the reaction system. It requires the reaction system to be anhydrous, low temperature, and A large amount of organic solvent is used, and hydrogen is generated, the reaction conditions are harsh, the operation is complicated, and the cost of raw materials is high, so it is not suitable for industrial scale production; the third is to use NaOH as a reaction catalyst, sodium chloroacetate and isoamyl alcohol react to generate isoamyloxyacetic acid sodium, and then acidified to obtain amyloxyacetic acid, the reaction yield of this route is low, the reaction time is long, the post-treatment is difficult, and it is not suitable for industrial production

In addition, the acid catalyst sulfuric acid used in the esterification step is cheap as a traditional esterification catalyst, and the catalytic effect is better and has been used so far, but it seriously corrodes the equipment and pollutes the environment with acid-containing wastewater.

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