HCID 11845249, Verbindung → 6,7-dihydro-4H-pyrazolo[5,1-c][1,4]thiazine-2-carbaldehyde

HRID 2216573Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2216573
[N:1]1[N:9]2[C:4]([CH2:5][S:6][CH2:7][CH2:8]2)=[CH:3][C:2]=1[CH2:10][OH:11]>O=[Mn]=O.C(Cl)(Cl)Cl>[N:1]1[N:9]2[C:4]([CH2:5][S:6][CH2:7][CH2:8]2)=[CH:3][C:2]=1[CH:10]=[O:11]

Komponenten

4

Edukt 1

HCID 11845249HCID 11845249, Verbindung

Produkt 1

HCID 118471336,7-dihydro-4H-pyrazolo[5,1-c][1,4]thiazine-2-carbaldehyde

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 14801Manganese dioxideKatalysatorHCID 6212ChloroformLösungsmittel

Versuchsvorschrift

MnO2 (activated) (11.46 g) was added to the CHCl3 (135 mL) solution of (6,7-dihydro-4H-pyrazolo[5,1-c][1,4]thiazin-2-yl)methanol (2.31 g) and refluxed for 1 h under a nitrogen atmosphere. The reaction mixture was filtered through a pad of Celite. The filtrate was concentrated under a reduced pressure. The residue was applied to silica gel column chromatography, then the column was eluted with n-hexane-AcOEt (1/1). The titled compound was obtained as pale yellow crystals (1.78 g, 78%).

Aufarbeitung

  1. temperaturerefluxed for 1 h under a nitrogen atmosphere
  2. filtrationThe reaction mixture was filtered through a pad of Celite
  3. concentrationThe filtrate was concentrated under a reduced pressure
  4. washthe column was eluted with n-hexane-AcOEt (1/1)

Quellen und Nachweise

ORD-Eintrag
ord-1338391c4a894a4c8ff4923ee7fd6282
Quelldatensatz
uspto-grants-2006_09
Patentnummer
US07112582B2

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