ChemicalBook CAS DataBase List 3,5-Dinitrobenzoic acid

3,5-Dinitrobenzoic acid synthesis

12synthesis methods

Product Name:3,5-Dinitrobenzoic acid
CAS Number:99-34-3
Molecular formula:C7H4N2O6
Molecular Weight:212.12

3,5-Dinitrobenzoic acid is synthesized by nitration of benzoic acid. Sulfuric acid was added to the dry reaction pot, and benzoic acid was added under stirring. Heat to 60°C, add fuming nitric acid dropwise, and complete the dropwise addition below 85°C. React at 80-85°C for 1 h, 100°C for 0.5-1h, and then heat up to 135°C for 2h. Leave overnight. The reaction solution was put into ice water to separate out crystals, filtered, washed with water and then washed with 50% ethanol to obtain 3,5-dinitrobenzoic acid. Yield 70%.

99-65-0 Synthesis

99-65-0
10 suppliers
$32.00/25g

124-38-9
130 suppliers
$214.00/14L

99-34-3
533 suppliers
$14.00/25g

Yield:99-34-3 65%

Reaction Conditions:

with Ti-mcm-41;ILTmCl₄ in N,N-dimethyl-formamide at 110; under 18751.9 Torr; for 10 h;Autoclave;Reagent/catalyst;Temperature;Pressure;

Steps:

2-7 Example 2

Add meta-dinitrobenzene (10mmol), Ti-MCM-41(at)ILTmCl4 (0.35g), DMF (20mL) into the stainless steel autoclave, then seal the reactor, and introduce carbon dioxide to remove the air in the reactor. Keep the carbon dioxide pressure at 2.5 MPa, and stir and react at 110°C for 10 hours. After the reaction is over, the materials are cooled, the excess CO2 is slowly released, the catalyst is at the bottom of the kettle, and the upper liquid containing the product is separated by filtration. The solvent is recovered from the product phase of the filtrate, and the crude product is recrystallized with ethanol and dried to obtain 3,5-dinitrobenzoic acid with a yield of 65% and a content of 96.4% (see Figure 2 for HPLC).

References:

CN113620808,2021,A Location in patent:Paragraph 0037-0048

65-85-0 Synthesis