Method for continuously producing 5-amino-1-amyl alcohol

A technology of amyl alcohol and amino group, which is applied in the field of continuous production of 5-amino-1-pentanol, can solve the problems of insufficient cleanliness and high efficiency in the production process, unfavorable large-scale industrial production, low yield of target products, etc., and achieves cheap production raw materials. Easy to obtain, reduce the investment of production equipment and production energy consumption, and have the effect of good life stability

Active Publication Date: 2019-04-26
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Also for example, Chinese patent CN108947851A discloses a method for preparing 5-amino-1-pentanol under milder reaction conditions by using cheap and easily available dihydropyran as a raw material through two-step reactions of hydration and ammoniation. However, this method is a batch reaction, and the reaction product and the catalyst need to be separated by centrifugation or filtration. The production efficiency is low, and the catalyst reuse operation is cumbersome and the effect is poor, resulting in high production costs.
[0008] Obviously, the existing technical methods still have problems such as high production cost, not clean and efficient production process, harsh reaction conditions, and low yield of target products, which are not conducive to large-scale industrial production

Method used

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  • Method for continuously producing 5-amino-1-amyl alcohol

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Embodiment 1: Preparation of dihydropyran hydrate

[0038] Weigh dihydropyran and deionized water in a mass ratio of 1:2 to 1:9 and add them to a 2L reaction kettle, seal the kettle, and use N 2 After replacement, pressurize to 0.1-3MPa, raise the temperature to 60-140°C under rapid stirring, and react at this temperature for 0.5-20h. After cooling down, collect the reaction solution for later use. Table 1 shows the dihydropyran hydrate prepared under different conditions.

[0039] Table 1. Preparation of dihydropyran hydrate under different conditions and its amination performance

[0040]

[0041]

Embodiment 2

[0042] Embodiment 2: Preparation of supported nickel-based catalyst

[0043]Dissolve a certain amount of nickel salt and metal additive salt in water to make a solution, add the dried carrier, stir into a uniform mud, soak at room temperature for 12 hours, then dry at 110°C for 12 hours, and roast at 500°C for 3 hours. Tablet sieve catalyst particles of 20-40 mesh, fill 2mL (2.4g) in the fixed bed reactor. Finally, in a hydrogen atmosphere (flow rate: 80-100mL / min), the temperature was raised to 450°C and reduced for 4 hours to obtain an activated catalyst. The composition of the catalyst is shown in Table 2.

[0044] Table 2. Catalyst composition and amination performance of dihydropyran hydrate

[0045]

Embodiment 3

[0046] Example 3: Different catalysts catalyze the amination reaction performance of dihydropyran hydrate and ammonia water

[0047] The dihydropyran hydrate 3 prepared in Example 1 and 25% concentrated ammonia water were mixed evenly in a mass ratio of 1:1 and pumped into the reactor. 2 Pressure 3MPa, H 2 The volume ratio to the reaction liquid is 1200 and the feed volume space velocity is 10h -1 The amination reaction performance of different supported Ni-based catalysts was studied under the same conditions, and the samples after 6h stabilization were taken for gas chromatography analysis. From the results in Table 2, it can be seen that the yield of the target 5-amino-1-pentanol is between 79-93%, indicating that the catalyst synthesized by the present invention can efficiently catalyze the amination reaction of dihydropyran hydrate and ammonia water.

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Abstract

The invention discloses a method for continuously producing 5-amino-1-amyl alcohol. The method comprises the following step: carrying out a continuous reductive amination reaction on a mixed reactionsystem with a dihydropyran aquo-complex, ammonium hydroxide and a loaded type nickel catalyst in a fixed bed reactor, thereby obtaining the 5-amino-1-amyl alcohol. According to the method, the dihydropyran aquo-complex and the ammonium hydroxide which are low in price and easy to obtain are adopted as raw materials, a loaded type non-noble heavy nickel is adopted as the catalyst in the fixed bed reactor, continuous production of the 5-amino-1-amyl alcohol at a low reaction temperature and low hydrogen pressure is achieved, a reaction product is directly separated from the catalyst in the reaction process, independent filtration or centrifugation treatment is not needed, the catalyst is good in service life stability, the method is simple in operation and process, the production efficiencycan be remarkably improved, the production cost can be lowered, and on-scale industrial production can be facilitated.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, in particular to a method for continuously producing 5-amino-1-pentanol. Background technique [0002] Amino alcohol is an important bifunctional compound containing both hydroxyl and amino groups in its molecule. It is widely used in the synthesis of medicine and pesticides, and is also often used as a building block in organic synthesis. In addition, aminoalcohols are structural motifs of various natural product molecules, are often biologically active, and have high medicinal value. For example, Manzamine A is an alkaloid with good antitumor and antifungal activities, and the starting material for its synthesis is 5-amino-1-pentanol. With the popularization and application of Manzamine A drug, the demand for 5-amino-1-pentanol will increase. [0003] The commonly used preparation methods of amino alcohols include Grignard reagent addition method, halohydrin amino substitution method and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/00C07C215/08
CPCC07C213/00C07C215/08
Inventor 黄志威陈静李雪梅夏春谷
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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