A kind of synthetic method of biochemical preparation tmb

A synthesis method and preparation technology, applied in the field of biochemical preparation TMB synthesis, can solve the problems of lack of data support, no use value, no operability, etc.

Active Publication Date: 2020-10-30
JINGCHU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Chinese patent CN1056304 discloses a synthetic method of TMB: taking 2,6-dimethylaniline as a raw material and oxidizing it into an azo compound with red blood salt Then add zinc powder with ammonium chloride solution to reduce to benzidine: Finally, it is rearranged into TMB under the action of hydrochloric acid, but this method has no experimental data support and is inoperable
[0008] Then use sulfuric acid to rearrange to TMB, the yield of this method is 45.4%, also no experimental data support, no operability
Moreover, the oxidation of 2,6-dimethylaniline is a very complicated process, and the use of hydrogen peroxide oxidation requires a catalyst to improve the selectivity of the reaction, otherwise, in addition to obtaining will also produce and / or In addition to the complex oxidation of 2,6-dimethylaniline, the reduction to benzidine is not easy, and the rearrangement is even more complex, far from being as simple as reported in CN1056304 and Ru2086536
[0009] To sum up, among the above three TMB synthesis methods, the synthesis method disclosed in DE2540740 is more mature, but due to the use of bromine and Pd / C, the cost is high, while CN1056304 and Ru2086536 only briefly describe the principle and lack data support. Inoperable and therefore useless

Method used

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  • A kind of synthetic method of biochemical preparation tmb
  • A kind of synthetic method of biochemical preparation tmb
  • A kind of synthetic method of biochemical preparation tmb

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Experimental program
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Embodiment 1

[0036] 1. Synthesis of 2,2′,6,6′-azotetramethylaniline-N,N-dioxide:

[0037]

[0038] In a 2000ml reaction flask, add 290.4g 2,6-xylidine (light red, purity over 97%), 348g water, 59g sodium tungstate dihydrate and 615ml ether, stir evenly, cool down to 20°C, pour into the reaction flask Add 451ml of 30wt% hydrogen peroxide solution dropwise to the solution, add dropwise for 1h, control the temperature of the reaction bottle at 20-30°C during the dropwise addition, continue to insulate and stir the reaction for 8h after dropping, after the reaction is completed, cool down to 5°C, precipitate and filter , wash the filter cake 3 times with 96ml of cold diethyl ether, and dry it in the air to obtain 318.7g of 2,2′,6,6′-azotetramethylaniline-N,N-dioxide, reddish brown, mp134~135℃, purity 99.3%, yield 98%.

[0039] Its structural formula is as follows:

[0040]

[0041] Elemental analysis; C: 80.9; H: 7.3; N: 11.4%; -1 .

[0042] The ether in the filtrate can be reclaimed...

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Abstract

The invention discloses a synthesis method of a biochemical preparation TMB. The synthesis method includes following steps: synthesizing 1,2, 2', 6, 6'-azo tetratoluidine-N, N-dioxide; synthesizing 1,2, 2', 6, 6'-tetramethyl diphenylhydrazine; synthesizing 3,TMB (1 / 2)H2SO4; preparing 4,TMB 2HCl; preparing TMB. The synthesis method is simple in synthesis route, cheap and easy-to-obtain in raw material, low in synthesis cost and high in yield.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a synthesis method of a biochemical preparation TMB. Background technique [0002] The Chinese name of TMB is 3,3',5,5'-tetramethylbenzidine, and its structural formula is: [0003] [0004] TMB is mainly used in the field of biochemistry. Because of its small amount of use, there are not many patents for its synthesis method. In recent years, due to the rapid development of biopharmaceuticals, the amount of biopharmaceuticals has gradually increased, so the patents for their synthesis methods have continued to increase. [0005] German patent DE2540740 discloses a synthetic method of TMB: 4-bromo-2,6-xylaniline TMB is condensed into TMB under the action of Pd / C catalyst, quaternary ammonium salt and sodium formate. This method is currently the best method for synthesizing TMB, and the yield reaches 63%. [0006] Chinese patent CN1056304 discloses a s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/00C07C211/50
CPCC07C209/00C07C209/54C07C241/02C07C291/08C07C211/50C07C243/22
Inventor 胡莉萍孟庆荣胡冠丰
Owner JINGCHU UNIV OF TECH
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