StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Hydrazine hydrate (1:1) → HCID 178420845, Verbindung

HRID 2359057
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2359057
C[N:2](C)[CH:3]=[CH:4][C:5]([C:7]1[S:8][CH:9]=[CH:10][CH:11]=1)=O.O.[NH2:14]N>C(O)C>[S:8]1[CH:9]=[CH:10][CH:11]=[C:7]1[C:5]1[CH:4]=[CH:3][NH:2][N:14]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 6023993-(Dimethylamino)-1-(2-thienyl)-2-propen-1-one

Produkt 1

HCID 178420845HCID 178420845, VerbindungAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 3-(dimethylamino)-1-(2-thienyl)prop-2-en-1-one (193 mmol) and hydrazine hydrate (396 mmol) in 50 mL ethanol was refluxed for 18 h and then allowed to cool to room temperature. The solvent was evaporated under reduced pressure and the residue was partitioned between ethyl acetate and water. The organic phase was successively washed with saturated aqueous ammonium chloride solution, saturated aqueous sodium bicarbonate solution and brine, dried over MgSO4, filtered and concentrated. The residue was recrystallized (dichloromethane/cyclohexane) to afford 26.0 g 3-(2-thienyl)-1H-pyrazole (90% yield).

Aufarbeitung

  1. temperaturewas refluxed for 18 h
  2. customThe solvent was evaporated under reduced pressure
  3. customthe residue was partitioned between ethyl acetate and water
  4. washThe organic phase was successively washed with saturated aqueous ammonium chloride solution, saturated aqueous sodium bicarbonate solution and brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue was recrystallized (dichloromethane/cyclohexane)

Quellen und Nachweise

ORD-Eintrag
ord-e2be4d0c5c224445817bd88c623ed731
Quelldatensatz
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08685974B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion