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Preparation method of 1,2-cyclopentanedicarboximide

A technology of cyclopentadiimide and formamide, applied in 1 field, can solve the problems of complicated purification operation, environmental pollution and the like, and achieve the effects of simple process, convenient purification and reduction of side reactions

Active Publication Date: 2021-02-12
内蒙古源宏精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The above reaction uses a large amount of phosphoric acid, which pollutes the environment, and the purification operation is complicated

Method used

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  • Preparation method of 1,2-cyclopentanedicarboximide
  • Preparation method of 1,2-cyclopentanedicarboximide
  • Preparation method of 1,2-cyclopentanedicarboximide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: Add 40g of cyclopentane-1-carboxamide-2-ammonium formate and 200ml of acetic anhydride to the reaction flask, raise the temperature to reflux, keep the reaction at 120°C for 6 hours, concentrate the acetic anhydride to dryness under reduced pressure, and add while hot Heat 100g of toluene to dissolve completely, add 100ml of water, keep warm at about 50°C for 1 hour, separate the water layer, cool the toluene layer to 5°C, filter, and dry to obtain the finished product of 1,2-cyclopentadicarboximide. Yield 92.1%, content 94.5%.

Embodiment 2

[0027] Example 2: Add 60g of cyclopentane-1-carboxamide-2-ammonium formate and 200ml of acetic anhydride to the reaction flask, raise the temperature to reflux, keep the reaction at 120°C for 6 hours, concentrate the acetic anhydride to dryness under reduced pressure, and add while hot Heat 100g of toluene to dissolve completely, add 100ml of water, keep warm at about 50°C for 1 hour, separate the water layer, cool the toluene layer to 5°C, filter, and dry to obtain the finished product of 1,2-cyclopentadicarboximide. Yield 90.8%, content 96.5%.

Embodiment 3

[0028] Example 3: Add 50g of cyclopentane-1-carboxamide-2-ammonium formate and 200ml of acetic anhydride to the reaction flask, raise the temperature to reflux, keep the reaction at 120°C for 6 hours, concentrate the acetic anhydride to dryness under reduced pressure, and add while hot Heat 100g of toluene to dissolve completely, add 100ml of water, keep warm at about 50°C for 1 hour, separate the water layer, cool the toluene layer to 5°C, filter, and dry to obtain the finished product of 1,2-cyclopentadicarboximide. Yield 95.0%, content 99.5%.

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Abstract

The invention relates to a preparation method of 1,2-cyclopentanedicarboximide. The method comprises the following steps: adding cyclopentane-1-formamide-2-ammonium formate and acetic anhydride into areaction bottle, heating to reflux, carrying out heat preservation reaction, concentrating acetic anhydride under reduced pressure to dryness, adding toluene while hot, heating to completely dissolve, adding water, keeping the temperature for a period of time, removing a water layer, cooling a toluene layer, filtering, and drying to obtain a 1,2-cyclopentanedicarboximide finished product. According to the method, phosphoric acid is not needed, the production period is short, the reaction process temperature is low, side reactions are greatly reduced, and the yield can reach 95%.

Description

Technical field: [0001] The invention relates to a preparation method of 1,2-cyclopentadicarboximide, which belongs to the field of chemical industry. Background technique: [0002] Gliclazide is the second-generation sulfonylurea oral hypoglycemic agent, which has the dual effects of lowering blood sugar and improving blood coagulation function. It is suitable for non-insulin-dependent diabetes and has been widely used clinically. The key intermediate in its synthesis The body is 1,2-cyclopentadiimide. Present production technology mainly contains to be that raw material synthesizes imide under high temperature condition with 2-carbamoyl ammonium cyclopentacarboxylate, and reaction formula is as follows: [0003] [0004] Also have in the prior art by 1,2-cyclopentadicarboxylic anhydride and ammonia are raw material synthetic imide, and reaction formula is as follows: [0005] [0006] Wherein the first preparation method has a shorter technical process than the sec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/52
CPCC07D209/52
Inventor 王兵波张森王伟张晓弟宋立雪
Owner 内蒙古源宏精细化工有限公司