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CAS No. : | 54709-94-3 | MDL No. : | MFCD09743644 |
Formula : | C5H6N2O | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | MMDFKVYPOQFQHP-UHFFFAOYSA-N |
M.W : | 110.11 | Pubchem ID : | 327041 |
Synonyms : |
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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 |
---|---|---|
87% | With potassium permanganate; sulfuric acid; at 45℃; for 1.0h; | Example 386-Oxo-1,6-dihydro-pyridazine-4-carboxylic acid The title compound from Example 37 (0.90 g, 8.2 mmol) was stirred in concentrated sulfuric acid (13 mL) and heated to 45 C. Potassium permanganate (3.6 g, 12 mmol) was added portion wise over 30 min to avoid letting the temperature rise. The reaction was allowed to stir for a further 30 min at 45 C. The reaction was then cooled to room temperature and ice was added to the reaction mixture. The resulting precipitate was collected by vacuum filtration, washing with cold water and diethyl ether to give 0.98 g (87%) of the title compound as the a pale green solid.1H NMR (300 MHz, CDCl3): delta (ppm) 13.39 (broad s, 1H), 8.12 (s, 1H), 7.22 (s, 1H). |
87% | With potassium permanganate; sulfuric acid; at 45℃; for 1.0h; | 6-Oxo-l,6-dihydro-pyridazine-4-carboxylic acidThe title compound from Example 18.2 (0.90 g, 8.17 mmol) was stirred in concentrated sulfuric acid (13 mL) and heated to 45 0C. Potassium permanganate (3.6 g, 12.25 mmol) was added portion wise over 30 min to avoid letting the temperature rise. The reaction was allowed to stir for a further 30 min at 45 0C. The reaction was then cooled to r.t. and ice was added to the reaction mixture. The resulting precipitate was collected by vacuum filtration, washing with cold water and diethyl ether to give 0.978 g (87%) of the title compound as the a pale green solid. 1H NMR (300 MHz, CDCl3) delta 13.39 (br, IH), 8.12 (s, IH), 7.22 (s, IH). |
77% | Example 306-Oxo-1,6-dihydro-pyridazine-4-carboxylic acid To a stirred solution of the title compound of Example 29 (4.4 g, 40 mmol) in concentrated sulphuric acid (80 mL), potassium dichromate (18 g, 61 mmol) was added in small quantities at 50-60 C. as a finely ground powder. The starting material was added to the mixture within 20 min. Stirring was continued for a further 10 min at 60 C., then the viscous green mixture was poured on crushed ice. The solid powder, which separated, was collected, washed with cold water and dried to give the title compound (4.5 g, 77%).1H NMR (400 MHz, (CD3)2SO): delta (ppm) 7.22 (s, 3H), 8.13 (s, 1H), 13.38 (s, broad, 1H). |
77% | With dipyridinium dichromate; sulfuric acid; at 50 - 60℃; for 0.5h; | Step 14B: 6-Oxo-1H-pyridazine-4-carboxylic acid; To a stirred solution of the subtitle compound of Step 14A (4.4 g, 40 mmol) in concentrated sulphuric acid (80 mL), potassium dichromate (18 g, 61 mmol) was added in small quantities at 50-60 C. as a finely ground powder. The starting material was added to the mixture within 20 min. Stirring was continued for a further 10 min at 60 C., then the viscous green mixture was poured on crushed ice. The solid powder, which separated, was collected, washed with cold water and dried to give the subtitle compound (4.5 g, 77%).1H NMR (400 MHz, (CD3)2SO): delta 7.22 (s, 3H), 8.13 (s, 1H), 13.38 (s, broad, 1H). |
77% | With potassium dichromate; sulfuric acid; at 50 - 60℃; for 0.5h; | Step 10B: 6-Oxo-1,6-dihydropyridazine-4-carboxylic acid; To a stirred solution of the subtitle compound of Step 10A (4.4 g, 40 mmol) in concentrated sulphuric acid (80 mL), potassium dichromate (18 g, 61 mmol) was added in small quantities at 50-60 C. as a finely ground powder. The starting material was added to the mixture within 20 min. Stirring was continued for 10 min at 60 C., the viscous green mixture was poured on crushed ice. The solids were filtered off and washed with cold water. After drying in vacuo the subtitle compound was isolated (4.5 g, 77%).1H NMR (400 MHz, DMSO-d6): delta 7.22 (s, 3H), 8.13 (s, 1H), 13.38 (s, broad, 1H). |
77% | With potassium dichromate; sulfuric acid; at 50 - 60℃; for 0.5h; | Step 7B: 6-Oxo-1,6-dihydropyridazine-4-carboxylic Acid To a stirred solution of the subtitle compound of Step 7A (4.4 g, 40 mmol) in concentrated sulphuric acid (80 mL), potassium dichromate (18 g, 61 mmol) was added in small quantities at 50-60 C. as a finely ground powder. The starting material was added to the mixture within 20 min. Stirring was continued for a further 10 min at 60 C., then the viscous green mixture was poured on crushed ice. The solid powder, which separated, was collected, washed with cold water and dried to give the subtitle compound (4.5 g, 77%).1H NMR (400 MHz, (CD3)2SO): delta 7.22 (s, 3H), 8.13 (s, 1H), 13.38 (s, broad, 1H). |
77% | With potassium dichromate; sulfuric acid; at 60℃; for 0.166667h; | Step 13B: 6-Oxo-1,6-dihydropyridazine-4-carboxylic acid To a stirred solution of the subtitle compound of Step 13A (4.4 g, 40 mmol) in concentrated sulphuric acid (80 mL), potassium dichromate (18 g, 61 mmol) was added in small quantities at 50-60 C. as a finely ground powder. The starting material was added to the mixture within 20 min. Stirring was continued for a further 10 min at 60 C., the viscous green mixture was poured on crushed ice. The solids were filtered off and washed with cold water. After drying in vacuo the subtitle compound was isolated (4.5 g, 77%). 1H NMR (400 MHz, (CD3)2SO): delta 7.22 (s, 3H), 8.13 (s,1H), 13.38 (s, broad, 1H). |