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Preparation method of 1, 2-cyclopentadicarboximide

The technology of cycloglutarimide and cycloglutarimide is applied in the field of preparation of 1,2-cycloglutarimide, and can solve the problems of easy coking, safety, low yield and the like, Achieve the effect of reducing production costs and safety hazards, good thermal stability and chemical stability, and reducing environmental pollution problems

Pending Publication Date: 2022-03-22
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

[0003] The existing preparation methods of 1,2-cyclopentadicarboxamide mainly include: 1. 1,2-cyclopentadicarboxamide is directly reacted at a high temperature of 300°C to synthesize 1,2-cyclopentadicarboxamide Amine, process coking phenomenon is serious, product yield is low (less than 50%), and quality is poor; -cyclopentadicarboximide, this method produces a large amount of waste salts, and the equipment is severely corroded, and the yield is not high; in addition, a catalyst is introduced in the ring-closure reaction process, and a depolymerization agent is added during vacuum distillation to reduce polymerization However, due to the high boiling point of the product, high temperature distillation is unavoidable, especially in the later stage of distillation, the local overheating of the still wall will inevitably cause coking or even carbonization of some products
[0004] The application number is 201811074979.1, and the patent named a synthesis method of 1,2-cyclopentadiimide proposes to use heat transfer oil as a solvent, but there are the following problems: after cooling and crystallization, it needs to be heated in the crystallization solvent To dissolve and recrystallize at 70-110°C, the crystallization solvents used are all dangerous chemicals, which have potential safety hazards. At the same time, the process steps are complicated, and the cost of producing 1,2-cyclopentadicarboximide is also high; and the heating temperature Higher, also prone to coking problems

Method used

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  • Preparation method of 1, 2-cyclopentadicarboximide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1: Add 200ml of 1-methyl-3-octylimidazole hexafluorophosphate to the reaction kettle, the density of 1-methyl-3-octylimidazole hexafluorophosphate is 1.2345g / cm 3 , and stirred, and then in the process of stirring, put 100g of 1,2-cyclopentadicarboxamide, then heat up to 250°C, and keep the reaction at this temperature for 5h to obtain ammonia and 200g of the reaction mixture. Absorption: Cool 200g of the reaction mixture to 85°C, then add 200ml of water and stir for 1h to dissolve the reaction product 1,2-cyclopentadicarboximide into water, then stand at 85°C for 1h, and layer up and down , the lower layer is an ionic liquid, which can be recovered and used in the next ring-closure reaction, and the upper layer is an aqueous phase solution; send 200ml of the aqueous phase solution to the decolorization kettle and stir, then add 1g of activated carbon during the stirring process, and then heat Raise the temperature to 95°C, decolorize at this temperature for 1.5...

Embodiment 2

[0026] Example 2: Add 405ml of 1-methyl-3-octylimidazole hexafluorophosphate to the reaction kettle, the density of 1-methyl-3-octylimidazole hexafluorophosphate is 1.2345g / cm 3 , and stirred, and then in the process of stirring, put 100g of 1,2-cyclopentadicarboxamide, then heat up to 250°C, and keep the reaction at this temperature for 5h to obtain ammonia and 250g of the reaction mixture. Absorption: Cool 250g of the reaction mixture to 85°C, then add 100ml of water and stir for 1h to dissolve the reaction product 1,2-cyclopentadicarboximide into water, then stand at 85°C for 1h, and layer up and down , the lower layer is an ionic liquid, which can be recovered and used in the next ring-closure reaction, and the upper layer is an aqueous phase solution; send 100ml of the aqueous phase solution to the decolorization kettle and stir, then add 1g of activated carbon during the stirring process, and then heat Raise the temperature to 95°C, decolorize at this temperature for 1.5...

Embodiment 3

[0027] Example 3: Add 200ml of 1-methyl-3-octyl imidazole hexafluorophosphate to the reaction kettle, the density of 1-methyl-3-octyl imidazole hexafluorophosphate is 1.2345g / cm 3 , and stirred, and then in the process of stirring, put 100g of 1,2-cyclopentadicarboxamide, then heat up to 250°C, and keep the reaction at this temperature for 5h to obtain ammonia and 200g of the reaction mixture. Absorption; cool down 200g of the reaction mixture to 85°C, then add 100ml of water and stir for 1h to dissolve the reaction product 1,2-cyclopentadicarboximide into water, then let it stand at 85°C for 1h, and layer up and down , the lower layer is an ionic liquid, which can be recovered and used in the next cyclization reaction, and the upper layer is an aqueous phase solution; send 100ml of the aqueous phase solution to the decolorization kettle and stir, then add 0.5g of activated carbon during the stirring process, and then Heat up to 95°C, decolorize at this temperature for 1.5h, p...

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Abstract

The invention discloses a preparation method of 1, 2-cyclopentadicarboximide, which sequentially comprises the following steps: (1) cyclization reaction; (2) dissolving and layering; (3) decoloring and filter pressing; (4) cooling and crystallizing; and (5) separating and drying. The preparation method of 1, 2-cyclopentadicarboximide provided by the invention has the beneficial effects that the ionic liquid is adopted to ensure that reactants and products have a good flowing state in the whole reaction process, so that heat transfer is uniform, local overheating is avoided, and coking and coking in the reaction are avoided; the production cost and the potential safety hazard are reduced, and meanwhile, the problem of coking during heating is avoided; the method is simple, and the prepared 1, 2-cyclopentadicarboximide product is good in quality and high in yield.

Description

Technical field: [0001] The patent of the present invention relates to a preparation method of 1,2-cyclopentadicarboximide, in particular to a preparation method of 1,2-cyclopentadicarboximide. 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. [0003] The existing preparation methods of 1,2-cyclopentadicarboxamide mainly include: 1. 1,2-cyclopentadicarboxamide is directly reacted at a high temperature of 300°C to synthesize 1,2-cyclopentadicarboxamide Amine, process coking phenomenon is serious, product yield is low (less than 50%), and quality is poor; -cyclopentadicarboximide, this method produces a large amount of waste salts, and the equipment is severely corroded, ...

Claims

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Application Information

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IPC IPC(8): C07D209/52
CPCC07D209/52Y02P20/54
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