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Microwave synthesis method for tri(2,2'-diphenol) biphosphite

A technology of bis-tri- and tri-alkyl phosphite is applied in the field of preparation of bis-phosphite ligands and achieves the effects of environmental friendliness, no pollution, solvent-free operation and simple post-treatment.

Active Publication Date: 2014-01-15
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This new process involves replacing three chemicals with two different types of molecules called trimethyltiophosphonium (TMP). By doing this we can create better products that are more efficient than traditional methods like dichlormorate or chloroforming reactions. These processes have fewer side products compared to previous techniques such as monochiorobutane dibromaldehyde(MBDBA), which were previously used for producing TOPOZOLINIDES. Additionally, these novel procedures allow us to produce other compounds without harmful substances from certain starting material sources while also being able to use less expensive equipment during production.

Problems solved by technology

This technical problem addressed in this patented technology relates to finding ways to efficiently produce high purity chemical compounds from biaryltriglycerides without generating unwanted side products or requiring excessively expensive equipment for separation purposes.

Method used

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  • Microwave synthesis method for tri(2,2'-diphenol) biphosphite

Examples

Experimental program
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Embodiment 1

[0020] Put 16.6 grams of triethyl phosphite, 18.6 grams of 2,2'-biphenol and 1.7 grams of diphenyl phosphorus chloride catalyst in a microwave reaction device, mix and stir evenly, and then react under microwave radiation with a power of 200w for 15 Minutes, after the completion of the reaction, the reaction crude product was recrystallized with a mixed solvent of toluene and n-hexane to obtain white crystals, which were verified by H NMR spectrum, phosphorus spectrum and high performance liquid chromatography, and the product was bisphosphite tris(2,2' -biphenol) ester, the yield is 90% (the yield is calculated based on 2,2'-biphenol).

Embodiment 2

[0022] Put 49.8 grams of triethyl phosphite, 18.6 grams of 2,2'-biphenol and 0.7 grams of phenylphosphorus dichloride catalyst in a microwave reaction device, mix and stir evenly, and react under microwave radiation with a power of 200w for 15 Minutes, after the completion of the reaction, recrystallize the crude product with acetonitrile to obtain white crystals, which are verified by H NMR spectrum, phosphorus spectrum and high performance liquid chromatography, and the product is tris(2,2'-biphenol) bisphosphite , the yield is 92% (the yield is calculated based on 2,2'-biphenol).

Embodiment 3

[0024] Put 24.8 grams of trimethyl phosphite, 18.6 grams of 2,2'-biphenol and 4.3 grams of diphenyl phosphorus chloride catalyst in a microwave reaction device, mix and stir evenly, and then react under microwave radiation with a power of 500w for 10 minutes, after the reaction was completed, the crude product of the reaction was recrystallized with a mixed solvent of ethyl acetate and sherwood oil to obtain white crystals, which were verified by proton nuclear magnetic resonance spectrum, phosphorus spectrum and high performance liquid chromatography, and the product was bisphosphite tris(2, 2'-biphenol) ester, the yield is 95% (the yield is calculated based on 2,2'-biphenol).

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Abstract

The invention discloses a microwave synthesis method for tri(2,2'-diphenol) biphosphite. The method comprises the following steps: taking trialkyl phosphate and 2,2'-diphenol as raw materials according to a molar ratio of 1:1-10:1, taking aryl-substituted phosphoric chloride or alkyl-substituted phosphoric chloride as a catalyst, and synthesizing the tri(2,2'-diphenol) biphosphite under solvent-free microwave radiation conditions, wherein the microwave radiation power is 100-1000W, and the microwave reaction time is 5-30 minutes. The process has the characteristics of high biphosphite yield, less byproducts, short reaction time, solvent-free operation, environment friendliness, zero pollution, simple after-treatment and the like.

Description

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Claims

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Application Information

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Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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