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ChemicalBook CAS DataBase List 3-Nitrophthalic anhydride
641-70-3

3-Nitrophthalic anhydride synthesis

10synthesis methods
3-Nitrophthalic anhydride can be prepared by heating 3-nitrophthalic acid under various conditions and by the action of acetic anhydride, essentially as in the procedure described. The direct nitration of phthalic anhydride yields 3-nitrophthalic anhydride together with the isomeric 4-nitro compound.
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Yield:641-70-3 98.9%

Reaction Conditions:

with thionyl chloride;N,N-dimethyl-formamide in cyclohexane at 5 - 10; for 3.83333 h;Reflux;Vilsmeier Reaction;Time;Reagent/catalyst;Solvent;Temperature;

Steps:

2 Example 2

3-Nitrophthalic acid (20 g, 94.7 mmol), cyclohexane (50 mL), catalyst DMF was added to the reaction flask.(0.5 mL); cool to 5 ° C with an ice bath, add thionyl chloride (16.8 g, 0.15 mmol) dropwise, stir the reaction at 10 ° C for 50 min, addThe temperature was raised by heating and reacted under reflux for 3 h. After the reaction was completed, the solvent n-heptane was recovered under reduced pressure. The product is dried by infrared light and light greenThe color solid was 3-nitrophthalic anhydride 18.1 g, and the yield was 98.9%.

References:

CN108727319,2018,A Location in patent:Paragraph 0021; 0023; 0024; 0026; 0028; 0030; 0033

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