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Synthesizing method of cis-1,2,3,6-tetrahydrophthalimide

A technology of tetrahydrophthalimide and phthalimide, which is applied in the direction of organic chemistry, can solve the problems of difficult application in the field of biology and materials science, low product quality, difficult separation, etc., and achieve Avoid polymerization side reaction, high conversion rate, high selectivity effect

Inactive Publication Date: 2018-08-17
仪征市海帆化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After testing, the multi-impurity structure contains double bonds, making it difficult to separate
[0009] When 1,2,3,6-tetrahydrophthalic anhydride and ammonia water, which contain a large amount of double-bond compound impurities, are subjected to amidation reaction at high temperature, it is inevitable to generate a large amount of It is difficult to separate the jelly, the product quality is low, and it is difficult to apply to the fields of biology and materials science

Method used

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  • Synthesizing method of cis-1,2,3,6-tetrahydrophthalimide

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0034] Add 30 g (0.20 mol) of phthalimide, 600 ml of N,N-dimethylformamide and 9 g of Raney nickel into a 1 L stainless steel magnetically stirred autoclave, and seal the autoclave. After the air in the kettle was replaced with nitrogen, stirring was started to raise the temperature.

[0035] When the temperature rises to 110°C, the gauge pressure is 0MPa. At this time, hydrogen gas was introduced, and the temperature in the kettle was ensured to be between 105-115°C. After 70 minutes, the pointer of the pressure gauge is raised, the hydrogen inlet valve is closed, and the heat preservation and stirring are continued for 30 minutes, and the pressure gauge returns to zero.

[0036] Re-open the hydrogen inlet valve, and after 2 hours, the pointer of the pressure gauge rises, close the hydrogen inlet valve, continue to keep warm and stir for 30 minutes, and the pressure gauge returns to zero.

[0037] In this way, whenever the pressure gauge has pressure, stop the hydrogen flow...

example 2

[0041] Add 30 g (0.37 mol) of phthalimide, 600 ml of N,N-dimethylformamide and 5 g of Raney nickel into a 1 L stainless steel magnetically stirred autoclave, and seal the reaction kettle. After the air in the kettle was replaced with nitrogen, stirring was started to raise the temperature.

[0042] When the temperature rises to 110°C, the gauge pressure is 0MPa. At this time, hydrogen gas was introduced, and the temperature in the kettle was ensured to be between 105-115°C. After 1 hour, the pointer of the pressure gauge is raised, the hydrogen inlet valve is closed, and the heat preservation and stirring are continued for 40 minutes, and the pressure gauge returns to zero.

[0043] Re-open the hydrogen inlet valve, and after 45 minutes, the pointer of the pressure gauge rises, close the hydrogen inlet valve, continue to keep warm and stir for 30 minutes, and the pressure gauge returns to zero.

[0044] In this way, whenever the pressure gauge has pressure, stop the hydrogen...

example 3

[0048] Add 30 g (0.37 mol) of phthalimide, 600 ml of N,N-dimethylformamide and 5 g of Raney nickel into a 1 L stainless steel magnetically stirred autoclave, and seal the autoclave. After the air in the kettle was replaced with nitrogen, stirring was started to raise the temperature.

[0049] When the temperature rises to 80°C, the gauge pressure is 0MPa. At this time, hydrogen gas was introduced, and the temperature in the kettle was ensured to be between 80-85°C. After 20 minutes, the pointer of the pressure gauge is raised, the hydrogen inlet valve is closed, and the heat preservation and stirring are continued for 20 minutes, and the pressure gauge returns to zero.

[0050] Re-open the hydrogen inlet valve, and after 18 minutes, the pointer of the pressure gauge rises, close the hydrogen inlet valve, continue to keep warm and stir for 20 minutes, and the pressure gauge returns to zero.

[0051] In this way, whenever the pressure gauge has pressure, stop the hydrogen flow...

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Abstract

The invention discloses a synthesizing method of cis-1,2,3,6-tetrahydrophthalimide. The cis-1,2,3,6-tetrahydrophthalimide is prepared by allowing phthalimide and hydrogen serving as the raw materialsto have reaction under the effect of a catalyst. The synthesizing method has the advantages that side reaction is avoided by changing process conditions, and high selectivity and high conversion rateof the reaction are achieved; the product with the content being 98% or above can be obtained by performing simple distillation and crystallization and filtering on reaction liquid; low-temperature reaction is achieved by adding Raney nickel serving as the catalyst to catalyze the reaction, and the reaction conversion rate can reach up to 97% or above.

Description

technical field [0001] The invention belongs to the improvement of the synthesis method of cis-1,2,3,6-tetrahydrophthalimide. Background technique [0002] Cis 1,2,3,6-tetrahydrophthalimide, the molecular structure is: [0003] [0004] Cis-1,2,3,6-tetrahydrophthalimide, also known as cis-1,2,3,6-tetrahydrophthalimide, is a white needle-like crystalline powder. As an organic synthesis intermediate, it is widely used in various fields of organic synthesis. It can be used in the synthesis of fungicide captan, and can also be used in the production of unsaturated resin. The product is used in insulating paint, insulating film and other industries, and has a wide application prospect. . [0005] At present, it is reported in open literature that its synthetic method is mostly to use maleic anhydride and 1,4-butadiene to carry out conjugate addition first to obtain 1,2,3,6-tetrahydrophthalic anhydride, and then add ammonia or The amidation reaction of urea yields the produc...

Claims

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Application Information

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IPC IPC(8): C07D209/48
CPCC07D209/48
Inventor 邹从伟戴久坤周芬沈永刚邹从欢
Owner 仪征市海帆化工有限公司
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