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Cyclopentane1,2-diimide preparation method

A technology of diimide and cyclopentane, which is applied in the field of cyclopentane 1, can solve the problems of carbonization, high raw material cost, and low total yield, and achieve the effects of reducing time and cost, increasing yield, and reducing pollution

Active Publication Date: 2006-12-13
ZHEJIANG JIUZHOU PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The main disadvantage of this method is that when converting from acid to acid anhydride, the raw material used is acetic anhydride, and when the acid anhydride is purified by distillation under reduced pressure, there will be carbonization under high temperature conditions, and the total yield is low and the cost of raw materials is high.

Method used

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  • Cyclopentane1,2-diimide preparation method

Examples

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Effect test

Embodiment 1

[0017] To form a salt, put 500g of 95% ethanol and 100g of cyclopentane 1,2-dicarboxamide into a 1000ml reaction bottle, heat it to 40-55°C to dissolve, add 147g of phosphoric acid dropwise after the dissolution is complete, and precipitate the material into a salt, drop After adding, keep warm for 30 minutes at 40-55°C, then cool with cold water, then cool with ice-salt water to an internal temperature of about 10°C, keep warm for 30 minutes, finish the heat preservation, spin dry by centrifuge, dry in a drying room, and dry to obtain About 225g of amine salt, the consumption of ethanol is 68g.

[0018] For cyclization, put 200g of the amine salt obtained above into a 500ml reaction bottle, and heat it with oil to dissolve the cyclization, heat to an internal temperature of 220-250°C and keep it warm for 2 hours to complete the cyclization reaction. Put the ammonium phosphate in the lower layer, the upper layer is cyclopentane 1,2-imide, and then after refining with toluene, ...

Embodiment 2

[0022] Get 100g of cyclopentane 1,2-dicarboxamide and 128g of 98% sulfuric acid, adopt the method as described in Example 1 to obtain 225g of amine salt, and the yield of amine salt is 100%. Then, the obtained amine salt was cyclized at 260° C. to obtain 66.82 g of cyclopentane 1,2-diimide with a total yield of 74.99%.

Embodiment 3

[0024] Get 100g of cyclopentane 1,2-dicarboxamide and 131g of 36% hydrochloric acid, adopt the method as described in Example 1 to obtain 136g of amine salt, and the yield of amine salt is 92.5%. Then, the obtained amine salt was cyclized at 225° C. to obtain 56.8 g of cyclopentane 1,2-diimide with a total yield of 63.75%.

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Abstract

The invention relates the organic synthesis method, especially the preparing method of cyclopentane 1, 2- diimide. The method comprises the following steps: dissolving the cyclopentane 1, 2-diformamide in organic solvent, then it reacting with acid salt, and getting the cyclopentane 1, 2- diimide. The invention has the characters of modifying the technology and improving the productivity. The invention has the advantages of reducing the preparing time, raw material, cost and pollution.

Description

technical field [0001] The invention relates to an organic synthesis method, in particular to a preparation method of cyclopentane 1,2-imide. Background technique [0002] Existing synthetic cyclopentane 1,2-diimide method is to take cyclopentane 1,2-dicarboxamide as raw material, through sodium hydroxide hydrolysis, refine cyclopentane 1,2-dicarboxylic acid, this The first-step reaction yield is 78%. Cyclopentane 1,2-dicarboxylic acid is converted to acetic anhydride and acid anhydride, and then purified by vacuum distillation. The acid anhydride is purified by passing through ammonia under toluene as a solvent. The yield in the second step is 73.92 %, if the raw material cyclopentane 1,2-dicarboxamide is used to calculate the yield is only 57.66%. [0003] [0004] The main disadvantage of this method is that when converting from acid to acid anhydride, the raw material used is acetic anhydride, and when the acid anhydride is purified by distilla...

Claims

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Application Information

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IPC IPC(8): C07D235/26
Inventor 戴兆云
Owner ZHEJIANG JIUZHOU PHARM CO LTD
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