HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 69217820, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | 6-Chloro-3-oxo-2,3-dihydropyridazine-4-carboxylic acid | HCID 334015 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 69217820 | HCID 69217820 | — |
Reaction Steps
Oxalyl chloride was added to a solution a 8.73 g of 6-chloro-3-oxo-2,3-dihydro-pyridazine-4-carboxylic acid and 1 ml DMF in 250 ml THF at 5-10° C. and the mixture was stirred at room temperature for 2 h. Afterwards, it was evaporated to dryness, the residue dissolved in 450 ml THF and 13.8 g potassium carbonate and a solution of 7.2 g 4-chloro-benzyl amide in THF were added. The solvent was distilled off after 2 h of stirring at room temperature, the residue suspended in 100 ml water and a pH of 6.4 was adjusted. The obtained precipitate was sucked off, suspended again in 50 ml water and the pH is adjusted to 3. Afterwards, the precipitate was sucked off and dried over phosphorous pentoxide in an desiccator.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07462613B2 |
| Source dataset | uspto-grants-2008_12 |
| ORD ID | ord-32ce09f7a451463297a40f72715d129d |
| Source note | uspto-grants-2008_12 |