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Microwave synthesis method for tri(3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-diphenol) biphosphite

A technology of trialkyl phosphite and bisphosphite, which is applied in the field of microwave synthesis of bisphosphite triester to achieve the effects of less by-products, high product yield and simple post-treatment

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

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Problems solved by technology

[0005] The object of the present invention is to provide a kind of microwave synthesis method of bisphosphite tris (3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-biphenol) ester, in order to solve Adopting phosphorus trichloride in the prior art is a series of problems that raw material brings

Method used

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  • Microwave synthesis method for tri(3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-diphenol) biphosphite
  • Microwave synthesis method for tri(3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-diphenol) biphosphite

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Embodiment 1

[0020] 14.5 grams of triethyl phosphite, 37.4 grams of 3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-biphenol and 2.7 grams of diphenyl phosphorus chloride catalyst In the microwave reaction device, after mixing and stirring evenly, react under the microwave radiation with a power of 200w for 25 minutes. After the reaction is completed, the reaction crude product is recrystallized with a mixed solvent of toluene and n-hexane to obtain the product. And HPLC analysis and verification, it is bisphosphite tris(3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-biphenol) ester with a yield of 90% (yield The rate is calculated based on 3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-biphenol).

Embodiment 2

[0022] 46.7 grams of triethyl phosphite, 37.4 grams of 3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-biphenol and 1.0 grams of phenyl phosphorus dichloride catalyst In a microwave reaction device, mix and stir evenly and react under microwave radiation with a power of 300w for 20 minutes. After the reaction is completed, the crude product is recrystallized with toluene and n-hexane to obtain the product. Liquid chromatography analysis verification, is bisphosphite tris (3,3'-di-tert-butyl-5,5'-dimethoxyl-2,2'-biphenol) ester, yield 89% (yield in 3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-biphenol as the basis for calculation).

Embodiment 3

[0024] 25.4 grams of trimethyl phosphite, 37.4 grams of 3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-biphenol and 6.2 grams of diphenyl phosphorus chloride catalyst In a microwave reaction device, mix and stir evenly and react under microwave radiation with a power of 500w for 15 minutes. After the reaction is completed, the reaction crude product is recrystallized with a mixed solvent of ethyl acetate and petroleum ether to obtain the product. Phosphorus spectrum and HPLC analysis verification, bisphosphite tris(3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-biphenol) ester, yield 91% (The yield is calculated based on 3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-biphenol).

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Abstract

The invention discloses a microwave synthesis method for tri(3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-diphenol) biphosphite. The method comprises the following steps: taking trialkyl phosphate and 3,3'-di-tert-butyl-5,5'-dimethoxy-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(3,3'-di-tert-butyl-5,5'-dimethoxy-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

technical field [0001] The invention relates to a microwave synthesis method of bisphosphite tris(3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-biphenol). Background technique [0002] Bisphosphite tris(3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-biphenol) ligand contains two coordinated phosphorus atoms in the molecular structure, which can be combined with transition Metal catalysts coordinate to form double-chelate-coordinated metal complexes, which play an important role in transition metal-catalyzed reactions. [0003] The synthesis method disclosed in the prior art is mainly divided into two steps: (1) Phosphorus trichloride reacts with 3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-biphenol to form 3,3'-di-tert-butyl-5,5'-dimethoxy-2,2'-bisphenoxyphosphine chlorine intermediate; (2) This intermediate is then combined with 3,3'-di-tert-butyl The base-5,5'-dimethoxy-2,2'-biphenol reacts under the action of an acid-binding agent to generate bisphosphite tris(3,3'-di-tert-butyl-5,5'-dimeth...

Claims

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Application Information

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IPC IPC(8): C07F9/6571
Inventor 蒋凌云李晨于海斌李继霞李俊郝婷婷
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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