A kind of preparation method of 4-aminobutanol

Abstract

The invention provides a method for preparing 4-aminobutanol, which uses phthalimide potassium salt and 4-chlorobutanol as raw materials, and prepares an intermediate in the presence of a solvent and a phase transfer catalyst , and then the intermediate is hydrolyzed under the action of an alkaline solution to obtain 4-aminobutanol. The raw materials used in the method are simple, the cost is low, the reaction conditions are mild, and there is no potential safety hazard. There is almost no additional reaction in the reaction process of various raw materials used; no difficult-to-separate substances are generated during the preparation process, and the post-treatment is simple and easy to operate; Therefore greatly improved the yield of 4-aminobutanol, improved the utilization rate of raw material, reduced production cost. That is, the yield of the product is obviously improved under the condition of low cost, and has remarkable economic benefits.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of 4-aminobutanol. [0002] technical background [0003] 4-Aminobutanol, the English name is 4-aminobutan-1-butanol, and its molecular weight is 89.14. It is an important pharmaceutical and chemical intermediate. Because it has active groups such as amino and hydroxyl groups at both ends of its molecule, it can further produce chemical reaction, introducing nitrogen atoms or other groups, so many domestic and foreign experts and scholars have done a lot of research on the preparation process of 4-aminobutanol. For the research of 4-aminobutanol, the experts initially prepared 4-aminobutanol by one-step reaction of azide compound. This method can be completed in one step, but there are certain hidden dangers of explosion and the yield is low; -Halogenated butyronitrile is used as a raw material, the nitrile group is reduced to obtain an ...

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Problems solved by technology

For the research of 4-aminobutanol, the experts initially prepared 4-aminobutanol by one-step reaction of azide compound. This method can be completed in one step, but there are certain hidden dangers of explosion and the yield is low; -Halogenated butyronitrile is used as a raw material, the nitrile group is reduced to obtain an amino group, and the product is hydrolyzed under high temperature and strong alkali conditions, the reaction conditions are very harsh and the yield is low; in the 1990s, Stein et al. 4-aminobutanol is prepared by reductive amination of ene-1,4-diol. This method not only needs harsh conditions of high pressure, but also needs expensive rhodium acetate catalyst in the reaction process, that is, the preparation conditions are harsh, the cost is high, and the yield is high. Low; subsequently, Ma Nan et al. used 4-aminobutyric acid as a raw material to prepare 4-aminobutanol through Boc-protected amino group, reduction of carboxylic acid, and then removal of Boc. The method is complicated to operate, and the reactants used The raw material is highly toxic, and the total yield can reach 68%, that is, the method is complicated to operate and has highly toxic substances

In 2016, Zhao Hui et al. used 2,3-dihydrofuran as a raw material, first treated it with an acidic aqueous solution, and then directly reacted the obtained crude product with hydroxylamine hydrochloride to obtain 4-hydroxybutyl oxime, and then used Raney nickel as a catalyst Hydrogen reduction is carried out to prepare 4-aminobutanol. In this method, due to the presence of concentrated hydrochloric acid in the process of Raney nickel catalytic hydrogenation, the catalyst is easy to lose activity and greatly reduces the progress of the reaction, and the catalyst itself has natural safety hazards and cannot be used. for large-scale industrial production

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