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A kind of preparation method of 2-acetyl phenothiazine

A technology of acetyl phenothiazine and phenothiazine, which is applied in the field of preparation of 2-acetyl phenothiazine, can solve the problems of long time, complexity, and inconspicuous reaction phenomenon, and achieves the advantages of preventing reversible reaction and short reaction time. Effect

Active Publication Date: 2016-06-22
TAICANG YUNTONG BIOCHEM ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional method for synthesizing 2-acetylphenothiazine is very complicated, specifically under the action of an organic solvent, the reflux reaction is carried out, the reaction time is long, the reaction phenomenon is not obvious, and the organic solvent used is more harmful to the environment Seriously, it does not conform to the concept of green chemistry

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The preparation method of the 2-acetylphenothiazine of the present embodiment, comprises the steps:

[0022] (1) To prepare phenothiazine, mix 2.5mol diphenylamine, 2.5mol sulfur with 0.21g catalyst—aluminum trichloride, heat to melt, heat to 185°C under stirring, and pass in an inert gas—CO 2 , continue heating to 200°C, and cool to room temperature to obtain 520g of phenothiazine with a purity of 96%;

[0023] The method introduces an inert gas, which can effectively remove the hydrogen sulfide generated by the reaction, thereby preventing reversible reactions, and is beneficial to the yield and purity of the phenothiazine; among many inert gases, the effect of carbon dioxide is the best.

[0024] (2) 2-acetyl phenothiazine is prepared by reacting acetic acid, dimethylaniline and phenothiazine.

[0025] In step (2), the preparation process of 2-acetylphenothiazine is:

[0026] (2a) Add 1mol acetic acid and 1mol dimethylaniline in the proportioning ratio in the react...

Embodiment 2

[0029] The preparation method of the 2-acetylphenothiazine of the present embodiment, comprises the steps:

[0030] (1) To prepare phenothiazine, mix 2.5mol diphenylamine, 2.1mol sulfur and 0.423g catalyst, heat to melt, heat to 185°C under stirring, and pass in an inert gas——CO 2 , continue heating to 200°C, and cool to room temperature to obtain 550g of phenothiazine with a purity of 98%;

[0031] The catalyst used in this step is the mixture of iodine and active earth that the mol ratio is 1:1;

[0032] (2) 2-acetyl phenothiazine is prepared by reacting acetic acid, dimethylaniline and phenothiazine.

[0033] In step (2), the preparation process of 2-acetylphenothiazine is:

[0034] (2a) Add 1mol acetic acid and 1.1mol dimethylaniline to the reaction vessel according to the proportioning ratio, grind evenly, then add 1mol phenothiazine, continue grinding, monitor the reaction with TLC, until the phenothiazine has reacted completely, then the phenothiazine The raw materia...

Embodiment 3

[0037] The preparation method of the 2-acetylphenothiazine of the present embodiment, comprises the steps:

[0038] (1) To prepare phenothiazine, mix 2.5mol diphenylamine, 1.67mol sulfur and 0.8g catalyst—aluminum trichloride, heat to melt, heat to 190°C under stirring, and pass in an inert gas——N 2 , continue heating to 205°C, and cool to room temperature to obtain 600g of phenothiazine with a purity of 98%;

[0039] (2) 2-acetyl phenothiazine is prepared by reacting acetic acid, dimethylaniline and phenothiazine.

[0040] In step (2), the preparation process of 2-acetylphenothiazine is:

[0041] (2a) Add 1.1mol acetic acid and 1mol dimethylaniline into the reaction vessel according to the proportioning ratio, grind evenly, then add 1mol phenothiazine, continue grinding, monitor the reaction with TLC, until the phenothiazine has reacted completely, then the phenothiazine The raw material point disappears, the grinding is stopped, and the product is obtained;

[0042] (2b) ...

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PUM

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Abstract

The invention relates to a preparation method of 2-acetylphenothiazine, which comprises the following steps: (1) phenothiazine preparation: mixing diphenylamine, sulfur and a catalyst (the mole ratio of the diphenylamine to the sulfur is (1-1.5):1), stirring and heating to 185-190 DEG C, introducing inert gas, continuing heating to 200-205 DEG C, and cooling to obtain the phenothiazine; and (2) reacting acetic acid, dimethylaniline and the phenothiazine to obtain the 2-acetylphenothiazine. The phenothiazine prepared by the preparation method has high purity, the yield of the 2-acetylphenothiazine is high, and the preparation method is pollution-free.

Description

technical field [0001] The invention relates to a preparation method of 2-acetylphenothiazine, which belongs to the field of chemical synthesis. Background technique [0002] Phenothiazine is an important fine chemical product and raw material. Its structure contains N and S heteroatoms. Early phenothiazines were mainly used as raw materials for insecticides, insect repellants, and dyes. With the mass production of oxazine, its various derivatives are gradually synthesized and applied in different fields. [0003] First, its derivatives can be used as polymerization inhibitors. When producing and refining various monomers, phenothiazine is used as a process polymerization inhibitor to prevent monomer polymerization. In recent years, as the amount of methacrylate used as construction materials etc. and polyacrylate in disposable diapers has rapidly increased, the amount of phenothiazine has also increased. Secondly, phenothiazine and its derivatives can be used as antioxida...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D279/20
CPCC07D279/20
Inventor 张卫东
Owner TAICANG YUNTONG BIOCHEM ENG
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