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ChemicalBook CAS DataBase List 4-Nitrophthalic acid

4-Nitrophthalic acid synthesis

13synthesis methods
-

Yield:610-27-5 95%

Reaction Conditions:

with 1-butyl-3-methylimidazolium hydrogen sulfate;water at 60 - 65; for 2.45 h;Green chemistry;

Steps:

General procedure for the synthesis of carboxylic acids from nitriles
General procedure: Aromatic or aliphatic nitriles (2 mmol) were dissolved in 5 ml of [bmim]HSO4 and the reaction mixture was heated at 60-65 °C for 1-3 h. The progress of reaction was monitored by TLC. After completion of reaction, as checked by TLC, the reaction mixture was poured into water containing crushed ice. The product was precipitated out, filtered and dried. The yield of the final product was high (>90%) in all cases. All final products obtained were found sufficiently pure so it didn’t need further purification.The filtrate was concentrated under vacuum, washed with diethylether twice and concentrated under high vacuum. After proper drying under reduced pressure, approximately 95% ionic liquid was recovered from the reaction and compared with the original ionic liquid to check its authenticity. The efficiency of recovered ionic liquid in conversion of nitriles to acids was found unchanged in comparison to the original one and we reused it up to 5-6 cycles without any significant loss of its activity.

References:

Kumar, Satyanand;Dixit, Sandeep Kumar;Awasthi, Satish Kumar [Tetrahedron Letters,2014,vol. 55,# 28,p. 3802 - 3804] Location in patent:supporting information

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