Hydrochloric Acid → HCID 18441970, Verbindung

HRID 458447Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 458447
[N:1]1[C:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])=[CH:5][CH:4]=[C:3]([C:12]([O:14]CC)=[O:13])[N:2]=1.Cl>C(O)C.[OH-].[Na+].CCOCC>[CH2:10]([O:9][C:7]([C:6]1[N:1]=[N:2][C:3]([C:12]([OH:14])=[O:13])=[CH:4][CH:5]=1)=[O:8])[CH3:11]

Komponenten

6

Edukt 2

HCID 313Hydrochloric AcidHCID 9815937HCID 9815937, Verbindung

Produkt 1

HCID 18441970HCID 18441970, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 702EthanolLösungsmittelHCID 3283Diethyl EtherLösungsmittelHCID 14798Sodium HydroxideLösungsmittel

Versuchsvorschrift

To the diethyl 3,6-pyridazinedicarboxylate (5.0 g, 22.3 mmol) in 150 ml ethyl alcohol, 24.5 ml 1N NaOH was added. The mixture was stirred for 2 hours. The resulting salt was collected by filtration then was dissolved in minimum amount of water. The aqueous solution obtained was then acidified with 2N HCl in ether until the PH=2 and extracted with ethyl acetate. The combined extracts were washed with brine and dried over sodium sulfate. Removal of the solvent afforded 4.1 g of light yellowish oil. 1HNMR (400 MHz, CD3OD) δ 8.42 (s, 2H), 4.52 (q, 2H), 1.42 (t, 3H) ppm.

Aufarbeitung

  1. filtrationThe resulting salt was collected by filtration
  2. dissolutionthen was dissolved in minimum amount of water
  3. customThe aqueous solution obtained
  4. extractionextracted with ethyl acetate
  5. washThe combined extracts were washed with brine
  6. dry with materialdried over sodium sulfate
  7. customRemoval of the solvent
  8. customafforded 4.1 g of light yellowish oil

Quellen und Nachweise

ORD-Eintrag
ord-c84b8e4b32d3471e89a3ee32b61a6b33
Quelldatensatz
uspto-grants-2007_03
Patentnummer
US07189851B2

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