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ChemicalBook CAS DataBase List 2,4,5-Trichlorophenol
95-95-4

2,4,5-Trichlorophenol synthesis

11synthesis methods
2,4,5-Trichlorophenol is prepared indirectly, by the alkaline hydrolysis of 1,2,4,5-tetrachlorobenzene,because the direct chlorination of 2,5-dichlorophenol, difficult to achieve, proceeds with poor yield.
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Yield:95-95-4 75.8%

Reaction Conditions:

Stage #1:2,4,5-trichloroaniline with sulfuric acid;sodium nitrite in water at 8;Sandmeyer Reaction;
Stage #2: with copper(ll) sulfate pentahydrate at 80;Sandmeyer Reaction;

Steps:

3 (3) Phenol hydroxyl reaction on diazo:
The raw material 2,4,5-trichloroaniline 930 g is dissolved in a 30% sulfuric acid solution of 7920 g.A solution of 460 g of sodium nitrite and 1500 mL of water was added with stirring.During the dropwise addition, the reaction temperature was controlled at about 8 °C. After the addition, keep warm for a while,Prepared as a diazonium salt for use.In another reaction bottle, add 615 g of copper sulfate pentahydrate.30% sulfuric acid solution 2200 g. The control temperature is around 80 °C.Add the above diazonium salt dropwise, add the reaction, keep the reaction for a period of time, GC tracking,Until the reaction is complete. After the reaction is completed, it is allowed to cool and extracted with dichloroethane.Rotary steaming to obtain a pale yellow solid target706 g,The content is 97%, and the yield is 75.8%.

References:

Changzhou University;Chen Xingquan;Dong Yanmin CN109354570, 2019, A Location in patent:Paragraph 0010; 0011; 0013; 0014

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