Potassium thiocyanate → HCID 178527845, Verbindung

HRID 900731Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 900731
Cl.[NH2:2][CH2:3][C:4]([C:6]1[CH:11]=[CH:10][N:9]=[CH:8][CH:7]=1)=O.[S-:12][C:13]#[N:14].[K+]>O>[N:9]1[CH:10]=[CH:11][C:6]([C:4]2[N:14]=[C:13]([SH:12])[NH:2][CH:3]=2)=[CH:7][CH:8]=1

Komponenten

4

Edukt 2

HCID 516872Potassium thiocyanateHCID 222816172-Amino-1-pyridin-4-yl-ethanone dihydrochloride

Produkt 1

HCID 178527845HCID 178527845, VerbindungAusbeute 74,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

2-Amino-1-pyridin-4-yl-ethanone hydrochloride (0.75 g, 4.348 mMol) was dissolved in water (15 mL), and to clear yellow solution was added potassium thiocyanate (0.7 g, 7.203 mMol). The mixture was heated to reflux for 4.0 h during which period HPLC showed complete disappearance of starting material. On cooling to room temperature, a yellow solid precipitate formed, which was collected by filtration. The solid was then re-suspended in a saturated solution of NaHCO3 (30 mL), stirred at room temperature for 0.5 h, and the resulting free base thiol was collected by filtration. The solid was dried under vacuum to yield 576 mg (59%) of a fluorescent yellow solid. MS(ES) 178 (M+H)

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 4.0 h during which period HPLC
  3. customa yellow solid precipitate formed
  4. filtrationwhich was collected by filtration
  5. filtrationthe resulting free base thiol was collected by filtration
  6. customThe solid was dried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-ddff7a0be1664111a3fa3873a8a04194
Quelldatensatz
uspto-grants-2008_04
Patentnummer
US07361669B2

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