Dimethylformamide → HCID 69217820, Verbindung

HRID 2374782Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2374782
[C:1]([Cl:6])(=O)[C:2](Cl)=O.[Cl:7][C:8]1[CH:9]=[C:10]([C:15]([OH:17])=O)[C:11](=[O:14])[NH:12][N:13]=1.C[N:19]([CH:21]=O)C>C1COCC1>[Cl:6][C:1]1[CH:2]=[CH:11][C:10]([CH2:21][NH:19][C:15]([C:10]2[C:11](=[O:14])[NH:12][N:13]=[C:8]([Cl:7])[CH:9]=2)=[O:17])=[CH:9][CH:8]=1

Komponenten

5

Edukt 3

HCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 3340156-Chloro-3-oxo-2,3-dihydropyridazine-4-carboxylic acid

Produkt 1

HCID 69217820HCID 69217820, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  1. customAfterwards, it was evaporated to dryness
  2. dissolutionthe residue dissolved in 450 ml THF
  3. addition13.8 g potassium carbonate and a solution of 7.2 g 4-chloro-benzyl amide in THF were added
  4. distillationThe solvent was distilled off after 2 h
  5. stirringof stirring at room temperature
  6. dry with materialdried over phosphorous pentoxide in an desiccator

Quellen und Nachweise

ORD-Eintrag
ord-32ce09f7a451463297a40f72715d129d
Quelldatensatz
uspto-grants-2008_12
Patentnummer
US07462613B2

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