Production method for catalytically synthesizing galbanate spice by using solid acid

Abstract

The invention discloses a production method catalytically synthesizing galbanate spice by using solid acid. The production method comprises steps of: (1) with dichloroethane as a solvent and ethyl diazoacetate and isoamyl alcohol as initial raw materials, carrying out O-H insertion reaction under a solid catalyst under protection by nitrogen gas to obtain ethyl isopentoxyacetate, saponifying and acidifying the reaction product to obtain isopentoxyacetic acid; (2) carrying out condensation reaction on isopentoxyl acetic acid and allyl alcohol by taking solid acid as a catalyst to obtain a galbanate spice product. According to the method, isoamyl alcohol and ethyl diazoacetate are used as initial raw materials, and O-H insertion reaction and condensation reaction are performed to produce thegalbanate spice, so that the reaction time is greatly shortened, the technological process is relatively short, the raw materials are easy to obtain, and the total yield is increased; solid-liquid separation of the solid acid catalyst is realized by adopting an automatic backwashing filtering technology, the method has the advantages of no corrosion to equipment and simple post-treatment, and theproblems that the equipment is corroded by the existing liquid acid and the acid-containing wastewater pollutes the environment are solved.

Description

technical field [0001] The invention belongs to the technical field of perfume production, and in particular relates to a production method of solid acid catalyzed synthesis of glycopyrrolate perfume. 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. Synthesizing amyl amyl o...

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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.