HCID 21914731, Verbindung → HCID 21914837, Verbindung
Reaktionsgleichung
[OH:1][CH2:2][C:3]1[N:4]=[C:5]([NH:8][C:9](=[O:13])[O:10][CH2:11][CH3:12])[S:6][CH:7]=1>C(Cl)(Cl)Cl.CO.[O-2].[Mn+4].[O-2]>[CH:2]([C:3]1[N:4]=[C:5]([NH:8][C:9](=[O:13])[O:10][CH2:11][CH3:12])[S:6][CH:7]=1)=[O:1]Komponenten
Edukt 1
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 3
Versuchsvorschrift
To a mixed solution of ethyl 4-(hydroxymethyl)-1,3-thiazol-2-ylcarbamate (446 mg) in chloroform (30 ml) and methanol (3 ml) was added portionwise manganese (IV) oxide chemicals treated (1.92 g) at room temperature. After the mixture was stirred at the same temperature for 2 hours, then treated manganese (IV) oxide chemicals (250 mg) was added again to the solution, and it was stirred at 50° C. for 3 hours. Manganese (IV) oxide was removed by filtration and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (10 g) using a mixed solvent of hexane and ethyl acetate (4:1). The fractions containing the objective compound were collected and evaporated under reduced pressure to give colorless powder (470 mg, 106.4%).
Aufarbeitung
- additiontreated (1.92 g) at room temperature
- stirringwas stirred at 50° C. for 3 hours
- customManganese (IV) oxide was removed by filtration
- concentrationthe filtrate was concentrated under reduced pressure
- customThe residue was purified by column chromatography on silica gel (10 g)
- additionThe fractions containing the objective compound
- customwere collected
- customevaporated under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-d99145b84e0344b8b2e4497e0b87da62
- Quelldatensatz
- uspto-grants-2006_10
- Patentnummer
- US07125901B2
Notizen zur Reaktion
Wird geladen…