Hydrochloric Acid → 2-Ethylthio-6-n-propylimidazo[1,2-b]pyridazin-3-ylsulfonamide
Reaktionsgleichung
[H-].[Na+].[CH2:3]([SH:5])[CH3:4].Cl[C:7]1[N:8]=[C:9]2[CH:14]=[CH:13][C:12]([CH2:15][CH2:16][CH3:17])=[N:11][N:10]2[C:18]=1[S:19]([NH2:22])(=[O:21])=[O:20].Cl>CN(C=O)C.O>[CH2:3]([S:5][C:7]1[N:8]=[C:9]2[CH:14]=[CH:13][C:12]([CH2:15][CH2:16][CH3:17])=[N:11][N:10]2[C:18]=1[S:19]([NH2:22])(=[O:21])=[O:20])[CH3:4]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
Sodium hydride (60%, 0.73 g, 18.2 mmol) was suspended in DMF (10.0 ml) under ice-cooling, and ethanethiol (1.35 ml, 18.2 mmol) was added dropwise thereto, and the mixture was stirred at 0° C. for 2 hours. 2-Chloro-6-propylimidazo[1,2-b]pyridazin-3-ylsulfonamide (1.00 g, 3.64 mmol) was added thereto and heated at 110° C. for 2.5 hours under stirring. The reaction mixture was left, cooled, diluted with water and acidified by dropwise addition of conc. hydrochloric acid. The precipitated solids were collected by filtration and washed with water, and the solids were suspended in a mixed solvent of chloroform and ethyl acetate, and the insoluble solids were collected by filtration, and the solids were washed with chloroform to give the title compound as gray crystals. The yield was 0.45 g (41.2%).
Aufarbeitung
- temperaturecooling
- temperatureheated at 110° C. for 2.5 hours
- stirringunder stirring
- waitThe reaction mixture was left
- temperaturecooled
- filtrationThe precipitated solids were collected by filtration
- washwashed with water
- filtrationthe insoluble solids were collected by filtration
- washthe solids were washed with chloroform
Quellen und Nachweise
- ORD-Eintrag
- ord-a9e5bfeac39f43c9a212871060b6171c
- Quelldatensatz
- uspto-grants-2013_03
- Patentnummer
- US08399381B2
Notizen zur Reaktion
Wird geladen…