Carbon Disulfide → (1,3)Oxazolo(4,5-b)pyridine-2-thiol
Reaktionsgleichung
[OH:1][C:2]1[C:3]([NH2:8])=[N:4][CH:5]=[CH:6][CH:7]=1.[OH-].[K+].[C:11](=S)=[S:12]>CCO>[O:1]1[C:2]2[C:3](=[N:4][CH:5]=[CH:6][CH:7]=2)[NH:8][C:11]1=[S:12]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
3-Hydroxy-2-aminopyridine (2.00 g, 18.2 mmol) and potassium hydroxide (1.22 g, 21.8 mmol) were dissolved in carbon disulfide (15 mL) and EtOH (25 mL), and the reaction mixture was heated to reflux overnight. Upon cooling to rt, the reaction mixture was concentrated under reduced pressure. The resulting solid was suspended in 1 M aqueous HCl, collected by filtration, washed with water (2×) and air-dried. Further drying in a 35° C. vacuum oven gave 2.52 g (91%) of the title compound as a tan solid. LC-MS: RT=4.82 min., [M+H]+=153.1
Aufarbeitung
- temperatureto reflux overnight
- concentrationthe reaction mixture was concentrated under reduced pressure
- filtrationcollected by filtration
- washwashed with water (2×)
- customair-dried
- customFurther drying in a 35° C. vacuum oven
Quellen und Nachweise
- ORD-Eintrag
- ord-19e6337ddada4661bb84eebb88a950a1
- Quelldatensatz
- uspto-grants-2014_09
- Patentnummer
- US08822472B2
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