Preparation method of 2-hydroxyl-3-butylene-1-amine

Abstract

The invention discloses a preparation method of 2-hydroxy-3-butene-1-amine, that is, firstly adding trimethylsilyl-protected 2-hydroxy-3-butene-1-carbonitrile, ether and lithium hydride into a container Aluminum, reflux reaction under stirring, add Na2SO4 12H2O and ether to the resulting reaction solution, collect the supernatant after standing still, and rotary evaporate to obtain 2-hydroxyl-3-buten-1-amine protected by trimethylsilane, which is added to 2- Hydrochloric acid was added to hydroxy-3-butene-1-amine, and the reaction was stirred at room temperature. Diethyl ether was added to the obtained reaction liquid and then separated, and the obtained aqueous phase was concentrated by a rotary evaporator to obtain 2-hydroxy-3-butene-1- Add NaOH solution to the amine hydrochloride, extract with ether, collect the organic phase, dry it with anhydrous Na2SO4, and rotary evaporate to obtain 2-hydroxy-3-butene-1-amine. The preparation method has the advantages of low production cost, simpler operation, a product yield of 63-70%, and a purity of 97%.

Description

technical field [0001] The present invention relates to a kind of preparation method of aminoalcohol, more specifically relate to the preparation method of 2-hydroxyl-3-buten-1-amine. Background technique [0002] 2-Hydroxy-3-buten-1-amine is an important chemical intermediate, its structural formula is as follows figure 1 As shown, it is widely used in medicine, pesticide and other fields. There are currently three methods for its chemical synthesis. [0003] route one ( J. Am. Chem. Soc . 1950, 72 , 4792), the schematic diagram of the reaction route of its synthesis process is as follows figure 2 Shown: That is, 3,4-epoxy-1-butene and ammonia water are used as starting materials, but this synthetic route cannot be regioselectively ammonolyzed, and the 2-amino-3-buten-1-ol by-product The product is difficult to separate from the target product 2-hydroxy-3-buten-1-amine, resulting in extremely inconvenient post-treatment and extremely low reaction yield. [0004] rou...

AI Technical Summary

Problems solved by technology

[0007] Since there is always a part of the product that cannot be distilled from the crude product during vacuum distillation, the reaction yields of route two and route three are not high

And when the amount of reaction is small, the method for purifying by distillation under reduced pressure can not obtain purified product at all

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