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ChemicalBook CAS DataBase List 5-Nitroisophthalic acid

5-Nitroisophthalic acid synthesis

7synthesis methods
5-Nitrobenzene-1,3-Dicarboxylic Acid is used in the synthesis of Glycopyrrolate, a novel pharmaceutical compound based on PDE IV inhibitors; used in the treatment of respiratory complaints. 5-Nitroisophthalic acid can be synthesized in 4 steps from sulfuric acid by successive reactions with nitric acid, and then filter, wash and dry the residence to obtain this product.
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Yield:618-88-2 90%

Reaction Conditions:

with sulfuric acid;nitric acid at 50 - 75;Temperature;Concentration;

Steps:

1-10 Example 1
As shown in Figure 1, pump sulfuric acid and 65% concentrated nitric acid to temperature zone 1 (10°C) to form mixed acid; the flow rate of nitric acid is 2mL/min, and the flow rate of sulfuric acid is 2mL/min. Pump a sulfuric acid solution (12wt%) of isophthalic acid to warm zone 2 to preheat to 50°C with a flow rate of 10mL/min.Then, the sulfuric acid solution of isophthalic acid and the mixed acid are transported into a tubular reactor for nitration reaction (temperature zone 3,75°C), and the reaction residence time is 4 minutes.The reaction liquid flows out and enters the continuous stirring microreactor to quench with water (temperature zone 4,10C), the flow rate of pumped water is 15mL/min, and the quenching residence time is 5min. After the system reached a steady state, a 20-minute sample was collected.The effluent slurry was filtered, washed with water, and vacuum dried at 60 C to obtain 47.5 g of product with a purity of 99.2% and a yield of 90%.

References:

Suzhou Hande Chuanghong Biochemical Technology Co., Ltd.;Mao Zhongping;Zhu Tianqi;Chen Wei;Yang Shihai;Gao Hailong CN111995524, 2020, A Location in patent:Paragraph 0050; 0051

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