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ChemicalBook CAS DataBase List 2,4-Dichloro-5-nitrophenol

2,4-Dichloro-5-nitrophenol synthesis

11synthesis methods
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Yield: 89.6%

Reaction Conditions:

Stage #1:2,4-dichlorophenol with sulfuric acid at 80; for 2 h;Large scale;
Stage #2: with sulfuric acid;nitric acid in chloroform at 0 - 20;Large scale;
Stage #3: at 100 - 105; for 5 h;Large scale;

Steps:

1-3 Example 3
First, put the measured 625kg of dichlorophenol into a 3000L sulfonation and nitration kettle, and slowly drop 415kg of concentrated sulfuric acid into the kettle while stirring. After the dripping was completed, the reaction was kept at 80°C for 2h, and after the reaction was completed, 400L of chloroform was added to dissolve. Turn on the frozen brine and cool it down to 0°C. While stirring, the mixed acid was added dropwise to the kettle, and the temperature during the process of adding the mixed acid was controlled to not exceed 20°C. After the nitration reaction was completed, the temperature was lowered to 10°C. Add 400L of water to stand still, divide the lower waste water, add 900L of water, transfer the nitrated material after the reaction to the hydrolysis kettle with stirring, turn on the steam, control the temperature at 100105, after the chloroform is completely removed, at 100 The hydrolysis reaction is carried out at ~105°C for 5 hours. After the reaction is cooled down, filtered with suction and washed with water, the product is obtained. The yield of the product reaches more than 89.6% and the purity is more than 99.1%.

References:

CN112759519, 2021, A Location in patent:Paragraph 0010; 0029-0034

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