Reaktion #619794

ord-8c3eae7f7b7640aebe2cad5939df6888

Lösungsmittel

Reaktionsbedingungen

Temperatur
25°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenconcentrated under reduced pressure
  2. 2
    Sonstigeto give a solid which
  3. 3
    Sonstigewas recrystallized from ethanol

Vorschrift

5-(2-Methoxy-benzoyl)-5,6-dihydro-cyclopenta[b]thiophen-4-one (2.53 g, 8.3 mmol), hydrazine monohydrate (0.65 mL, 12 mmol), glacial acetic acid (1.5 mL) and ethanol (20 mL) were heated at 100° C. under nitrogen for 4 hr. The mixture was cooled to 25° C. and concentrated under reduced pressure to give a solid which was recrystallized from ethanol to provide the corresponding 6-(2-Methoxy-phenyl)-4,7-dihydro-1-thia-4,5-diaza-cyclopenta[a]pentalene (2 g, 7.4 mmol) as white solid in 89% yield.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08853207B2uspto-grants-2014_10