The synthetic method of triphenylmethane

A technology of triphenylmethane and a synthesis method, which is applied in chemical instruments and methods, hydrocarbons, hydrocarbons, etc., can solve the problems of long reaction time and difficulty in realizing industrial application, and achieves convenient post-processing and industrial application prospects. Considerable, high-yield effect

Inactive Publication Date: 2021-03-05
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method takes a long time to react and requires the use of organometallic catalysts, making it difficult to realize industrial application

Method used

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  • The synthetic method of triphenylmethane

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Experimental program
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Effect test

Embodiment 1

[0057] The synthetic method of embodiment 1, triphenylmethane, carry out following steps successively:

[0058] (1) Under the protection of an inert gas (nitrogen), add 23g (1mol) of sodium, 300mL of toluene, and 4mL of oleic acid to the reaction device, heat up to reflux (110°C) and stir, stop heating after reflux for 1h, and stir at high speed until Cool to room temperature.

[0059] (2), under the protection of inert gas (nitrogen), slowly drop 56g (0.5mol) chlorobenzene and 50mL toluene mixed solution in step (1) gained liquid, the temperature of control reaction system is not more than 40 during the dropping process ℃; After the dropwise addition, react at 30℃ for 2h.

[0060] (3), under the protection of an inert gas (nitrogen), slowly drop the liquid obtained in step (2) into a mixed solution of 10g (0.25mol) acetonitrile and 30mL toluene, and the time for dropping is 30min. The reaction was stopped at 10°C for 3h.

[0061] (4) Add 100 mL of 20% ammonium chloride aqueo...

Embodiment 2

[0065] The synthetic method of embodiment 2, triphenylmethane, carries out following steps successively:

[0066] (1), under the protection of an inert gas (nitrogen), add 23g (1mol) of sodium, 300mL of xylene, and 2g of sodium stearate into the reaction device, heat up to reflux (137°C) and stir, and stop heating after reflux for 1h. Stir on high speed until cool to room temperature.

[0067] (2), under the protection of inert gas (nitrogen), slowly drop 56g (0.5mol) chlorobenzene and 50mL xylene mixed solution in step (1) gained liquid, control the temperature of reaction system in the dropping process not to exceed 40°C; after the dropwise addition, react at 30°C for 2h.

[0068] (3), under the protection of an inert gas (nitrogen), slowly drop the liquid obtained in step (2) into a mixed solution of 8g (0.2mol) acetonitrile and 30mL xylene, the time for the addition is 30min, after the addition is completed Keep the reaction at 10°C for 3h, then stop.

[0069] (4) Add 1...

Embodiment 3

[0072] The synthetic method of embodiment 3, triphenylmethane, carries out following steps successively:

[0073] (1) Under the protection of an inert gas (nitrogen), add 23g (1mol) of sodium, 300mL of toluene, and 4mL of oleic acid to the reaction device, heat up to reflux (110°C) and stir, stop heating after reflux for 1h, and stir at high speed until Cool to room temperature.

[0074] (2), under the protection of inert gas (nitrogen), slowly drop 78.5g (0.5mol) bromobenzene and 80mL toluene mixed solution in the liquid obtained in step (1), control the temperature of the reaction system in the dropping process not to exceed 40°C; after the dropwise addition, react at 30°C for 2h.

[0075] (3), under the protection of an inert gas (nitrogen), slowly drop the liquid obtained in step (2) into a mixed solution of 10g (0.25mol) acetonitrile and 30mL toluene, and the time for dropping is 30min. React at 10°C for 3h to stop the reaction.

[0076] (4) Add 100 mL of 20% ammonium ...

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Abstract

The invention discloses a synthesis method of triphenylmethane, which comprises the following steps in sequence: under the protection of an inert gas, adding higher fatty acid or higher fatty acid salt and sodium into an organic solvent; adding halogenated benzene and The mixed solution of organic solvent is reacted; the liquid obtained from the reaction is added dropwise to the mixed solution of acetonitrile and organic solvent to continue the reaction; Solvent, vacuum distillation to obtain triphenylmethane. By adopting the method of the present invention to synthesize triphenylmethane, the utilization rate of raw materials is high, the use of expensive catalysts is avoided, the emission of three wastes is reduced, and the production cost is reduced. At the same time, the product has high purity and high yield, and has good industrial application value. .

Description

technical field [0001] The present invention relates to the synthetic method of organic compound triphenylmethane. Background technique [0002] Triphenylmethane is an important fine chemical intermediate, mainly used in environmental protection catalysts, photoinitiators, pharmaceutical intermediates, acid dyes, etc. [0003] At present, there are many synthetic methods for triphenylmethane, mainly four kinds: [0004] 1. Synthesis method of phenylboronic acid. Literature (Beilstein Journal of Organic Chemistry, 2016, 12, 496-504) uses chlorobenzene as a solvent to synthesize triphenylmethane from phenylboronic acid and diphenylmethanol under the catalysis of copper (II) trifluoromethanesulfonate, and the reaction yield is 78%. The reaction raw material price of this method is higher than that of the product, and a metal salt catalyst is used, the post-treatment is inconvenient, and it is difficult to realize industrial application. [0005] 2. Grignard reagent synthesi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C2/86C07C15/16
CPCC07C2/861C07C15/16
Inventor 陈新志毛崇智钱超
Owner ZHEJIANG UNIV
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