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A kind of method for preparing cyclic imide

A technology of cyclic imide and cyclic acid, which is applied in the field of organic chemical synthesis, can solve the problems of unfavorable industrial production, unfriendly environment, and low yield, and achieve the effects of easy industrial production, environmental friendliness, and high reaction yield

Active Publication Date: 2017-08-25
江西天新药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a method for preparing cyclic imides in order to overcome the disadvantages of unfriendly environment, high cost, low yield and unfavorable industrial production caused by the methods for preparing cyclic imides in the prior art. The method does not use pyridine, which is not only environmentally friendly, low in cost, convenient to operate and easy for industrial production, but also has high reaction yield and good product quality

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  • A kind of method for preparing cyclic imide
  • A kind of method for preparing cyclic imide
  • A kind of method for preparing cyclic imide

Examples

Experimental program
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Effect test

Embodiment 1

[0031] This example is used to illustrate the method for preparing cyclic imides of the present invention.

[0032] Add 62.5g (0.177mol) cyclic acid, 38.1g (0.180mol) right amine, 800ml n-butanol and 0.2g (0.0032mol) boric acid in the 1000ml reaction tank with reflux water separator, stirring blade and thermometer, stir under 400rpm And heated to 120 ° C, keep the stirring speed and temperature constant to carry out the reflux water separation reaction, after 14 hours of reaction, recover 700ml of solvent under reduced pressure, then add 10ml of water while it is hot, stir and beat at 600rpm for 30min. Then circulate the water first, then cool the material to 8°C, and stir at 300rpm for 40min. Discharge, filter and wash with 25g of water. After determination, the wet weight of the product was 104.0 g, and after drying, a white crystalline powder was obtained, and the dry weight was 90.1 g after weighing.

[0033] The white crystalline powder that present embodiment obtains i...

Embodiment 2

[0038] This example is used to illustrate the method for preparing cyclic imides of the present invention.

[0039]Add 62.5g (0.177mol) cyclic acid, 44.5g (0.210mol) right amine, 900ml n-butanol and 0.11g (0.00178mol) boric acid in the 1000ml reaction tank of band reflux water separator, stirring blade and thermometer, stir under 400rpm And heated to 80 ° C, keep the stirring speed and temperature constant to carry out the reflux water separation reaction, after 16 hours of reaction, recover 800ml of solvent under reduced pressure, then add 10ml of water while it is hot, stir and beat for 30min at 500rpm. Then circulate water first, then cool water to cool the material to 5° C., and stir at 300 rpm for 0.5 hour. Discharge, filter and wash with 25g of water. After determination, the wet weight of the product was 102g, and after drying, a white crystalline powder was obtained, and the dry weight was 88g after weighing.

[0040] The white crystalline powder that present embodim...

Embodiment 3

[0043] This example is used to illustrate the method for preparing cyclic imides of the present invention.

[0044] Add 62.5g (0.177mol) cyclic acid, 30.0g (0.142mol) right amine, 500ml n-butanol and 1.05g (0.017mol) boric acid in the 1000ml reaction tank of band reflux water separator, stirring blade and thermometer, stir under 400rpm And heated to 140 ° C, keep the stirring speed and temperature constant to carry out the reflux water separation reaction, after 12 hours of reaction, recover 400ml of solvent under reduced pressure, then add 10ml of water while it is hot, stir and beat at 600rpm for 30min. Then circulate water first, then cool water to cool the material to 10° C., and stir at 300 rpm for 1 hour. Discharge, filter and wash with 25g of water. After determination, the wet weight of the product was 103g, and after drying, a white crystalline powder was obtained, and the dry weight was 89g after weighing.

[0045] The white crystalline powder that present embodime...

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Abstract

The invention relates to the field of organic chemical synthesis, and discloses a method for preparing cyclic-imide. The method comprises the following steps: mixing naphthenic acid, a D-amino-compound, an organic solvent and a catalyst for reaction, and after the end of the reaction, performing aftertreatment on the materials, so as to obtain the cyclic-imide, wherein the catalyst is boracic acid or a boracic acid derivative. The method does not adopt pyridine, and is environment-friendly, low in cost, convenient to operate, easy for industrial production, high in reaction yield, and excellent in product quality.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a method for preparing cyclic imides. Background technique [0002] Cyclic imide, i.e., cis-1,3-dibenzyl-5-[(1s,2s)-1,3-dihydroxy-1-(4-nitrophenyl)-propan-2-yl] -Tetrahydropyrrole[3,4-d]imidazole-2,4,6(5H)-trione is an important intermediate mainly used in the synthesis of biotin. [0003] In the existing process for synthesizing cyclic imides, US3876656 discloses the use of chiral auxiliary agents (1s, 2s)-(+)-threo-1-(4-nitrophenyl)-2-amino-1, 3-propanediol (the right amine) and 1,3-dibenzyl imidazolin-2-one (the cyclic acid) can be obtained by condensation dehydration reaction in toluene and pyridine. A large amount of pyridine is used in this method. Pyridine is a colorless or yellow liquid with a foul smell. Although it belongs to the low-toxicity category, its foul smell has a great impact on the human body and the production environment, and the large amount of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/04
CPCC07D487/04
Inventor 司玉贵郭军陈璋章根宝
Owner 江西天新药业股份有限公司
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