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One-pot method for synthesizing 3, 3'-diamino benzophenone

A technology of diaminobenzophenone and dinitrobenzophenone, which is applied in the field of 3,3'-diaminobenzophenone synthesis, can solve the problems of unsuitability for industrial production, severe reaction conditions, and high impurity content , to achieve the effect of reducing solvent cost and waste liquid production, high purity and high yield

Active Publication Date: 2019-03-01
宏威高新材料有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] One of the objectives of the present invention is to propose a method for one-pot synthesis of 3,3'-diaminobenzophenone, which solves the problems of the prior art in the synthesis of 3,3'-diaminobenzophenone Technical problems such as low yield, high impurity content, severe reaction conditions, long reaction cycle, high production of three wastes, high cost, and unsuitability for industrial production

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  • One-pot method for synthesizing 3, 3'-diamino benzophenone
  • One-pot method for synthesizing 3, 3'-diamino benzophenone
  • One-pot method for synthesizing 3, 3'-diamino benzophenone

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Embodiment 1

[0036] This embodiment provides a method for synthesizing 3,3'-diaminobenzophenone, specifically:

[0037] 25°C, add benzophenone 91g (0.5mol) to a 2L titanium alloy pressure reactor, then add 50g of HZSM-4 catalyst, solvent methylene chloride 200mL, stir to dissolve, add 550ml, 2mol / L of pentoxide Dinitrogen dichloromethane solution, stirred for 1h.

[0038] After the reaction, 2 grams of nickel powder was added, and hydrogen gas was introduced to make the pressure in the reactor reach 0.5 MPa, and the reaction was fully carried out for 1 hour while insulated and stirred.

[0039] After the reaction, the reaction solution was filtered, and the filtrate was evaporated to dryness under pressure to obtain a crude product of 3,3'-diaminobenzophenone. The crude product was recrystallized in a solution of ethanol: water = 1:2 to obtain white powdery crystals, and after drying, 80 g of refined 3,3'-diaminobenzophenone was obtained.

[0040] In this embodiment, the yield of 3,3'-di...

Embodiment 2

[0051] At 30°C, add 91g (0.5mol) of benzophenone into a 2L titanium alloy pressure reactor, then add 50g of HZSM-4 catalyst, solvent methylene chloride 200mL, stir and dissolve, then add 550ml, 2mol / L of pentoxide Dinitrogen dichloromethane solution, stirred for 5h.

[0052] After the reaction, 2 grams of nickel powder was added, and hydrogen gas was introduced to make the pressure in the reactor reach 1.5 MPa, and the reaction was carried out with insulation and stirring for 5 hours.

[0053] After the reaction, the reaction solution was filtered, and the filtrate was evaporated to dryness under pressure to obtain a crude product of 3,3'-diaminobenzophenone. The crude product was recrystallized in a solution of ethanol: water = 1:2 to obtain white powdery crystals, and after drying, 88.9 g of refined 3,3'-diaminobenzophenone was obtained.

Embodiment 3

[0057] At 28°C, add 91g (0.5mol) of benzophenone into a 2L titanium alloy pressure reactor, then add 50g of HZSM-4 catalyst, solvent methylene chloride 200mL, stir and dissolve, then add 550ml, 2mol / L of pentoxide Dinitrogen dichloromethane solution, stirring reaction 10h.

[0058] After the reaction, 2 grams of nickel powder was added, and hydrogen gas was introduced to make the pressure in the reactor reach 1 MPa, and the reaction was carried out with insulation and stirring for 10 hours.

[0059] After the reaction, the reaction solution was filtered, and the filtrate was evaporated to dryness under pressure to obtain a crude product of 3,3'-diaminobenzophenone. The crude product was recrystallized in a solution of ethanol: water = 1:2 to obtain white powdery crystals, and after drying, 86.7 g of refined 3,3'-diaminobenzophenone was obtained.

[0060] In this example, the yield of 3,3'-diaminobenzophenone was 81%, and the purity was 99.4%.

[0061] The melting point of th...

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Abstract

The invention discloses a one-pot method for synthesizing 3, 3'-diamino benzophenone, relates to the technical field of synthesis of diamino benzophenone, and solves a plurality of problems existing in the method for synthesizing 3, 3'-diamino benzophenone in the prior art. The method comprises the following steps of: using benzophenone as a raw material, adding benzophenone into a reactor, addinga catalyst and a solvent, stirring and dissolving, adding a dichloromethane solution of dinitrogen pentoxide, enabling benzophenone and dinitrogen pentoxide to react under the action of a catalyst togenerate an intermediate 3, 3'-dinitro benzophenone; After the reaction in the step 1 is finished, nickel powder is added into the reaction solution, and then hydrogen is introduced into the reactor,so that the intermediate 3, 3'-dinitrobenzophenone reacts with the hydrogen under the action of the nickel powder to generate 3, 3'-diamino benzophenone. The one-pot method for synthesizing 3, 3'-diamino benzophenone has the advantages of high yield, high purity, mild synthesis conditions, short synthesis period, less three-waste production, low cost and suitability for industrial production.

Description

technical field [0001] The invention relates to the technical field of 3,3'-diaminobenzophenone synthesis, in particular to a method for synthesizing 3,3'-diaminobenzophenone in one pot. Background technique [0002] 3,3'-diaminobenzophenone is the core raw material for the preparation of etherketone polyimide, and the bonding and peeling strength of the polyimide composite film prepared from this raw material to the copper clad laminate reaches 350Kg / M, which is a kind of Very good TPI adhesive film for flexible copper clad laminates, with very broad application prospects. This technology was first developed by Mitsui toatsu Chemicals Inc., due to the high preparation cost of 3,3'-diaminobenzophenone, TPI resin made from 3,3'-diaminobenzophenone The high price limits its widespread use. [0003] The literature Synthesis of aromatic compounds; Kagaku (Kyoto, Japan), 37(9), 706-9; 1982, discloses a kind of preparation of 3,3'- The method of diaminobenzophenone has many sid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/08C07C205/45C07C221/00C07C225/22
CPCC07C201/08C07C221/00C07C205/45C07C225/22
Inventor 不公告发明人
Owner 宏威高新材料有限公司
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