Unlock instant, AI-driven research and patent intelligence for your innovation.

Preparation method of glutaryl imide derivative

A technology of glutarimide and derivatives, which is applied in the field of compound preparation, can solve the problem of high cost of glutarimide, and achieve the effects of reducing production cost, improving efficiency and wide source of raw materials

Inactive Publication Date: 2021-03-30
南京德尔诺医药科技有限公司
View PDF6 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to provide a kind of preparation method of glutarimide derivative, to solve the high defect of synthetic glutarimide cost in the prior art

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0023] A preparation method of glutarimide derivatives, said method comprising the steps of:

[0024] Step 1: Under negative pressure, add acetic anhydride dropwise to molten 1,1-cyclohexyl diacetic acid to react to obtain 1,1-cyclohexyl diacetic anhydride:

[0025] Among them, the pressure in negative pressure state is -0.15~-0.08MPa;

[0026] The molar ratio of the 1,1-cyclohexyl diacetic acid and acetic anhydride is 1:1.4~2.0;

[0027] The dropping time of the acetic anhydride is 0.5~3h, and the dropping temperature is 110~130°C;

[0028] Step 2: Add ammonia water to the ammoniation kettle, add dropwise 1,1-cyclohexanediacetic anhydride to carry out the ammoniation reaction, add hydrochloric acid to adjust the pH value, and obtain the precipitated crystals as pentanepentamic acid:

[0029] Add 10-25 parts of ammonia water into the ammoniation kettle, add 1,1-cyclohexanediacetic anhydride dropwise to carry out the ammoniation reaction;

[0030] Add active carbon to the re...

Embodiment 1

[0038] Under negative pressure, with a pressure of -0.15MPa, add 14 parts of acetic anhydride dropwise to 10 parts of molten 1,1-cyclohexyl diacetic acid to react to obtain 1,1-cyclohexyl diacetic anhydride. is 0.5h, and the dropping temperature is 110°C;

[0039] Add 10 parts of ammonia water into the ammoniation kettle, add 1,1-cyclohexanediacetic anhydride dropwise to carry out the ammoniation reaction, and the reaction time is 1h;

[0040] Add 5 parts of activated carbon to the reaction solution, suction filter, add 10 parts of hydrochloric acid to adjust the pH value to acidic, after the crystals are precipitated, wash with deionized water and dry to obtain pentanepentamic acid;

[0041] Add pentanevaleramic acid, 20 parts of toluene solvent and 3 parts of glacial acetic acid into the reaction kettle, heat to 70°C and stir, reflux for 6 hours, stop heating and cool down to 10°C, and suction filter to obtain a filter cake;

[0042] The filter cake was added into 30 parts ...

Embodiment 2

[0045] Under negative pressure, with a pressure of -0.1MPa, add 18 parts of acetic anhydride dropwise to 10 parts of molten 1,1-cyclohexyl diacetic acid to react to obtain 1,1-cyclohexyl diacetic anhydride. For 2h, the dropping temperature is 120°C;

[0046] Add 18 parts of ammonia water into the ammoniation kettle, add 1,1-cyclohexanediacetic anhydride dropwise to carry out the ammoniation reaction, and the reaction time is 1.5h;

[0047] Add 5 parts of activated carbon to the reaction solution, suction filter, add 10 parts of hydrochloric acid to adjust the pH value to acidic, after the crystals are precipitated, wash with deionized water and dry to obtain pentanepentamic acid;

[0048] Add pentanevaleramic acid, 30 parts of toluene solvent and 4 parts of glacial acetic acid into the reaction kettle, heat to 75°C and stir, reflux for 7 hours, stop heating and cool down to 14°C, and suction filter to obtain a filter cake;

[0049] The filter cake was added into 50 parts of a...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a preparation method of a glutaryl imide derivative, which comprises the following steps: in a negative pressure state, dropwise adding acetic anhydride into molten 1, 1-cyclohexyl diacetic acid, and reacting to obtain 1, 1-cyclohexyl diacetic anhydride; adding ammonia water into an ammoniation kettle, dropwise adding 1, 1-cyclohexanediacetic anhydride to carry out ammoniation reaction, and adding hydrochloric acid to adjust the pH value, so as to obtain precipitated crystals, namely pentane valeric acid; adding pentane valeric acid, a toluene solvent and glacial aceticacid into the reaction kettle, heating, stirring, reacting, cooling, and carrying out suction filtration to obtain a filter cake; and adding the filter cake into ammonia water for soaking and stirring, carrying out suction filtration again, leaching with deionized water, and drying to obtain glutaryl imide. According to the preparation method of a glutaryl imide derivative, acetic anhydride and 1, 1-cyclohexyldiacetic acid are used as raw materials, so that the reaction efficiency is effectively improved, the product yield is increased, the production cost of the product is reduced, and producing benefits are improved.

Description

technical field [0001] The invention relates to the technical field of compound preparation, in particular to a preparation method of glutarimide derivatives. Background technique: [0002] There are many synthesis methods involving glutarimide derivatives in the prior art. For example, Chinese patent CN201880069719.7 and other patent documents have made a lot of disclosures about the synthesis technology of this product. However, since various intermediates are used for synthesis, the cost is high, the side reactions are many, and the utilization rate of raw materials is low. And adopt 1,1-cyclohexyl diacetic acid, acetic anhydride, ammonium acetate etc. reaction, the product that obtains will not be very high in content, and the main reason is that the content of product is not high and The problem of low yields. Therefore, in order to improve the utilization rate of raw materials, increase the yield and reduce the cost, it is necessary to improve the scheme. Contents ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/88C07D211/02
CPCC07D211/88C07D211/02
Inventor 许玉东徐飞翔
Owner 南京德尔诺医药科技有限公司