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Method for synthesis of N,N,N',N'-tetra(beta-hydroxypropyl)hexanediamide with carrier solid base catalyst

A technology of solid base catalyst and adipamide, applied in chemical instruments and methods, preparation of carboxylic acid amides, preparation of organic compounds, etc., can solve problems such as increased steric hindrance, difficult experimental conditions, and difficult rearrangement , to achieve the effect of reducing the content, high activity and selectivity, and accelerating the reaction

Inactive Publication Date: 2016-06-08
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since this method needs to use a special high-vacuum device to carry out vacuum distillation on excess raw materials, the experimental conditions are relatively strict, and the production cost is correspondingly high.
From the perspective of the reaction principle, it has been reported in the literature that this type of reaction first undergoes transesterification to form an oxazoline ring, and then rearranges it into an amide compound. Due to the presence of a methyl group, the steric hindrance becomes larger, and the rearrangement is not easy to carry out, so it is difficult. synthesis

Method used

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  • Method for synthesis of N,N,N',N'-tetra(beta-hydroxypropyl)hexanediamide with carrier solid base catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Preparation of 50% supported solid base catalyst

[0021] Take equal amounts of N,N,N',N'-tetrakis(β-hydroxypropyl)adipamide and sodium oxide, put them into a mortar, grind them, repeat 3 times, and then put them in an oven at 110°C Dry for 3 hours, take out, grind, and set aside.

Embodiment 2

[0023] Add 13.3g (0.10mol) of diisopropanolamine and 0.18g (accounting for 0.8% of the total material) of 50% NaOH / adipamide-loaded solid base, heated and stirred, heated to 145°C, and when the pressure was 0.05MPa, 8.7g (0.05mol) of dimethyl adipate was added dropwise, and the dripping was completed in 40 minutes. Stop the depressurization, and grind crushed solids.

[0024] Take out 2.3g without any treatment, directly dry to obtain 2.2g, yield 95.78%. The melting point is 115~122°C. Add 8 mL of absolute ethanol to the remaining 13.76 g, heat and stir until the solid becomes a fine slurry, stop the reaction, cool, filter with suction, and dry to obtain 12.5 g, yield 92.86%, melting point 118~121 °C.

Embodiment 3

[0026] Add 13.3g (0.10mol) of diisopropanolamine and 0.23g (accounting for 1.05% of the total material) of 50% NaOH / adipamide-loaded solid base, heated and stirred, heated to 145°C, and when the pressure was 0.05MPa, 8.7g (0.05mol) of dimethyl adipate was added dropwise, and the dripping was completed in 40 minutes. Stop the depressurization, and grind crushed solids. Add 10.2ml of absolute ethanol, heat, stir until completely dissolved, stop the reaction, cool, filter with suction, and dry to obtain the target product. The yield is 92.09%, and the melting point is 117~120°C.

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Abstract

The invention discloses a method for synthesis of N,N,N',N'-tetra(beta-hydroxypropyl)hexanediamide with a carrier solid base catalyst and relates to N,N,N',N'-tetra(beta-hydroxypropyl)hexanediamide synthesis methods. The method includes: adding diisopropanolamine and the solid base catalyst into a four-neck flask with a mechanical stirrer, a constant-pressure dropping funnel and a distiller; heating to 135-145 DEG C, dropwise adding dimethyl adipate, and continuing reaction for a period of time after dropping is finished; cooling after reaction, stirring while replenishing methyl alcohol to avoid agglomeration, and carrying out filtering, cold methanol washing and drying to obtain a white powder product. The method has the advantages of avoidance of equipment corrosion, easiness in product separation, product recyclability, waste reduction and the like, and a whole process is more environment friendly. In addition, the catalyst can increase base contact area to accelerate reaction, base content is reduced, and introduction of new media is avoided.

Description

technical field [0001] The invention relates to a method for synthesizing adipamide, in particular to a method for synthesizing N,N,N',N'-tetrakis(β-hydroxypropyl)adipamide with a solid base catalyst. Background technique [0002] At present, the synthesis method of N,N,N',N'-tetrakis(β-hydroxypropyl)adipamide mainly adopts the reaction of dimethyl adipate and diisopropanolamine to synthesize it. When reporting the synthesis of N,N,N',N'-tetrakis(β-hydroxyethyl)adipate diamide, the synthesis of this compound was attached, and excessive diisopropanolamine and dimethyl adipate were added , synthesized under the conditions of strong alkali, high temperature and high vacuum, and then use a high vacuum and high airtight device to distill the remaining diisopropanolamine and cool it to obtain the product. If there are special requirements for purity, further processing can be carried out. purification. However, because this method needs to use a special high-vacuum device to car...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C233/18
CPCC07C231/02C07C233/18
Inventor 孔祥文顾春玲王欢张静
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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