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Method for recycling byproducts in preparation process of iodosuccinimide

A technology of iodosuccinimide and preparation process, applied in the directions of iodine, iodine/hydrogen iodide, organic chemistry, etc., can solve problems such as unavailability of by-products, and achieve the effect of fast reaction

Active Publication Date: 2021-01-26
启东东岳药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] All the above processes will inevitably produce iodine bromide by-products, which cannot be utilized

Method used

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  • Method for recycling byproducts in preparation process of iodosuccinimide
  • Method for recycling byproducts in preparation process of iodosuccinimide
  • Method for recycling byproducts in preparation process of iodosuccinimide

Examples

Experimental program
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Effect test

Embodiment 1

[0018] 45 grams of iodine, 30 grams of bromosuccinimide, 270 milliliters of dichloroethane, heat preservation and reflux at 80-90 ° C for 6 hours, azeotropically distill 180 milliliters of solvent, add 120 milliliters of dichloroethane, and then Evaporate 120 ml of dichloroethane, add another 120 ml of dichloroethane, distill off 60 ml of solvent, cool to 10-15°C, filter with suction, and dry under reduced pressure to obtain iodosuccinimide. The titrated content was 99.2%.

[0019] Add 10% sodium hydroxide solution to the dichloroethane and iodine bromide solution (360ml) distilled off azeotropically, adjust the pH to 10-12, separate the phases, add hydrochloric acid to the aqueous phase to adjust the pH to 6-7, add sub Sodium bisulfate solution until the solution turns from dark red to light yellow, 27.5% hydrogen peroxide is added dropwise to precipitate iodine, and filtered to obtain 20 grams of crude iodine.

[0020] Add 20 grams of crude iodine to 100 milliliters of dich...

Embodiment 2

[0022] 18 grams of refined iodine products recovered in Example 1, 12 grams of bromosuccinimide, and 108 milliliters of dichloroethane were kept at 80-90° C. for reflux for 6 hours, and 72 milliliters of solvents were evaporated azeotropically. 48 milliliters of dichloroethane, then distilled 48 milliliters of dichloroethane, then added 48 milliliters of dichloroethane, and then distilled 24 milliliters of solvent, cooled to 10-15 ° C, suction filtered, and dried under reduced pressure to obtain iodo Succinimide. The titrated content was 99.3%.

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Abstract

The invention discloses a method for recycling byproducts in the preparation process of iodosuccinimide. The method comprises the following steps: recycling and refining the byproducts iodine bromidegenerated in the preparation process of iodosuccinimide into iodine, and preparing iodosuccinimide. The whole process is quick in reaction and suitable for industrial production.

Description

technical field [0001] The invention relates to a method for recycling by-products in the preparation process of iodosuccinimide. Background technique [0002] Iodosuccinyl is a common iodine reagent with stronger activity than iodine, potassium iodate, etc. It is widely used in the fields of pesticides, medicine and fine chemicals. The structure is as follows: [0003] [0004] The preparation method of iodosuccinimide is described in the literature Synthesis of N-iodosuccinimide and its application in H 2 SO 4 as efficient iodination reagent for deactivated aromatic compounds[J].Russian Journal of Organic Chemistry(2001),37(10),1503-1504 and CN201410188992.5 have reports, the above literature patents use iodine and bromosuccinimide as Starting material, the reaction yields iodosuccinimide. The reaction principle is as follows: [0005] [0006] Above technological process all can inevitably produce iodine bromide by-product, and this by-product cannot be utiliz...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/46C01B7/14
CPCC07D207/46C01B7/14
Inventor 龙中柱禹艳昆蔡畅蔡水洪
Owner 启东东岳药业有限公司
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