Dimethylamine → 2-t-butyl-4-chloro-5-dimethylamino-3(2H)-pyridazinone

HRID 1291219Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1291219
[C:1]([N:5]1[C:10](=[O:11])[C:9]([Cl:12])=[C:8](Cl)[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2].[CH3:14][NH:15][CH3:16]>C(O)C.O>[C:1]([N:5]1[C:10](=[O:11])[C:9]([Cl:12])=[C:8]([N:15]([CH3:16])[CH3:14])[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2]

Komponenten

4

Edukt 2

HCID 674DimethylamineHCID 27822252-Tert-butyl-4,5-dichloro-2,3-dihydropyridazin-3-one

Produkt 1

HCID 189188582-t-butyl-4-chloro-5-dimethylamino-3(2H)-pyridazinone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 19096565Water ethanolLösungsmittel

Versuchsvorschrift

In ethanol-water (2:1) (45 ml)was dissolved 2-t-butyl-4,5-dichloro-3(2H)-pyridazinone (4.4 g) followed by addition of 50% dimethylamine (7.2 g), and the mixture was stirred at room temperature for 15 hours. After removal of ethanol, the residue was extracted with diethyl ether and the organic layer was washed with saturated aqueous NaCl solution, dried over anhydrous magnesium sulfate, and concentrated to dryness. This residue was washed with n-hexane and dried. White powder, 4.4 g. 1H-NMR (CDCl3) δ: 1.63(9H,s), 3.10(6H,s), 7.57(1H,s).

Aufarbeitung

  1. customAfter removal of ethanol
  2. extractionthe residue was extracted with diethyl ether
  3. washthe organic layer was washed with saturated aqueous NaCl solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated to dryness
  6. washThis residue was washed with n-hexane
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-bd9b7dbfe91846e7a43003a5310b5e7e
Quelldatensatz
uspto-grants-1998_05
Patentnummer
US05753664

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