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Method for preparing 3,3'-(1,2-dioxethyl)bidiphenylamine

A technology of bis-diphenylamine and dioxyethyl, which is applied to the preparation of organic compounds, the preparation of amino hydroxyl compounds, chemical instruments and methods, etc., to achieve the effect of low cost

Inactive Publication Date: 2011-06-22
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The preparation method of 3,3'-(1,2-dioxyethyl)bis-diphenylamine has never been reported in the literature

Method used

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  • Method for preparing 3,3'-(1,2-dioxethyl)bidiphenylamine
  • Method for preparing 3,3'-(1,2-dioxethyl)bidiphenylamine

Examples

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Embodiment 1

[0018] Embodiment 1, a kind of preparation method of 3,3'-(1,2-dioxyethyl) diphenylamine, take aniline, resorcinol, 1,2-dibromoethane and sodium hydroxide as raw materials , follow these steps in order:

[0019] 1), preparation of m-hydroxydiphenylamine (with reference to "Journal of Jiangsu Institute of Technology" 2004, 16 (4): 30-32): 16.5g (0.15mol) resorcinol was reacted with 15mL aniline, and the reaction conditions were: Add 50 mL of xylene as a solvent, 1.8 mL of phosphoric acid with a mass fraction of 85% as a catalyst, drop aniline into the kettle within 1 hour at 139° C., and continue the reaction for 10 hours after dropping. The obtained reaction solution was separated into an organic phase, and the xylene in the organic phase was distilled off, and cooled to obtain m-hydroxydiphenylamine with a purity of 95%. The yield of m-hydroxydiphenylamine in this step was 75%.

[0020] 2), in the m-hydroxydiphenylamine obtained in step 1), add 75mL of toluene and 20mL (0.16...

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Abstract

The invention discloses a method for preparing 3, 3'-(1, 2 dioxygen ethyl) dual diphenylamine. The method comprises the following steps in turn: 1) aniline and m-dihydroxybenzene are reacted to generate m-hydroxyl diphenylamine; 2) salifying reaction is carried out, namely the m-hydroxyl diphenylamine, an alkali water solution and an organic solvent are subjected to azeotropic distillation in a reaction kettle, and aqueous phase is removed after the azeotrope is condensed, so that the organic solvent reflows to the reaction kettle; and 3) condensation reaction is carried out, namely, 1, 2-dibromoethane is added in the mixture of the m-hydroxyl diphenylamine salt and the organic solvent for reaction to generate the 3, 3'-(1, 2 dioxygen ethyl) dual diphenylamine. The 3, 3'-(1, 2 dioxygen ethyl) dual diphenylamine produced by the preparation method has the characteristics of low cost, mild reaction condition, and the like.

Description

technical field [0001] The invention relates to a preparation method of an organic compound 3,3'-(1,2-dioxoethyl)bis-diphenylamine. Background technique [0002] 3,3'-(1,2-dioxyethyl)bis-diphenylamine with the structural formula shown in formula 1 is a chemical synthesis intermediate, which is an intermediate in the synthesis of some biologically active substances, pesticides, medicines and other products body. [0003] [0004] Formula 1 [0005] The preparation method of 3,3'-(1,2-dioxyethyl)bis-diphenylamine has never been reported in the literature. Contents of the invention [0006] The technical problem to be solved by the present invention is to provide a method for preparing 3,3'-(1,2-dioxoethyl)bis-diphenylamine with low cost, mild reaction conditions and no catalyst. [0007] In order to solve the problems of the technologies described above, the present invention provides a kind of 3,3 '-(1,2-dioxyethyl) preparation method of diphenylamine, comprising the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/84C07C213/06
Inventor 陈新志周少东
Owner ZHEJIANG UNIV