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CAS No. : | 699-98-9 | MDL No. : | MFCD00005915 |
Formula : | C7H3NO3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | MCQOWYALZVKMAR-UHFFFAOYSA-N |
M.W : | 149.10 | Pubchem ID : | 69688 |
Synonyms : |
|
Chemical Name : | 2,3-Pyridinedicarboxylicanhydride |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogenchloride; In sodium hydroxide; acetonitrile; | EXAMPLE 1 Preparation of 2-(5-isopropyl-5-methyl-4-oxo-2-imidazolin-2-yl)nicotinic acid STR8 To a stirred suspension of 2,3-pyridinecarboxylic anhydride (30 g) in 150 mL of acetonitrile is added a solution of <strong>[40963-14-2]2-amino-2,3-dimethylbutyramide</strong> (28 g) in 140 mL of acetonitrile at 25 to 30 C. The mixture is stirred for 2 hours. The solvent is removed at 50 C. and reduced pressure. The residual gum is dissolved in 230 mL of 2.6N sodium hydroxide and heated to 80 C. for 1.5 hours. The mixture is cooled to 25 C. and acidified to a pH of 3 with 65 mL of 37% hydrochloric acid. The resulting solution is extracted with two 200 mL portions of methylene chloride. The extracts are concentrated to a residue of 33 g of the desired product, mp 160-165 C. After standing overnight, the aqueous layer deposits 3.8 g of the picolinic acid isomer, mp 155-157 C. (dec.). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
General procedure: A mixture of 10 mL methanolic solution of pyridine-2-carboxamide (0.3663 g, 3 mmol) and 10 mL methanolic solution of 4,4'-dimethoxy-2,2'-bipyridine (0.2162 g, 1 mmol) was stirred at room temperature for half an hour. Solution of EuCl3 was prepared by dissolving 1 mmol (0.2583 g) of EuCl3 in 10 mL of methanol and this solution was added to the ligands solution drop by drop with continuous stirring. The pH of resulting solution was maintained between 6 and 7. The reaction mixture was refluxed at 70 °C for 4 h. After refluxing for 4 h, the solution was cooled to room temperature and left as such overnight. Complex C1 was obtained as white precipitate which was filtered off, washed with methanol nd then dried under vacuum. The synthesis of complexes C2-C4 were done by adopting the same method as given above. Complex C2 was obtained from 3 mmol PCAO (0.3663 g), 1 mmol DMBP (0.2162 g) and1 mmol EuCl3 (0.2583 g), complex C3 was obtained from 3 mmol PDCA(0.4473 g), 1 mmol DMBP (0.2162 g) and 1 mmol EuCl3 (0.2583 g) and complex C4 was obtained from 3 mmol PM (0.3 mL), 1 mmol DMBP(0.2162 g) and 1 mmol EuCl3 (0.2583 g). |
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