Reaktion #81821

ord-85aae3c011414557809e137dd866b50d

Lösungsmittel

Reaktionsbedingungen

Temperatur
170°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling to room temperature the mixture
  2. 2
    Extraktionextracted with ethyl acetate
  3. 3
    WaschenThe organic phase was washed
  4. 4
    Sonstigedried
  5. 5
    Sonstigeevaporated

Vorschrift

A suspension of the 2-chloro-5,11-dihydro-11-ethyl-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (0.14 g) in 3-hydroxypyrrolidine (0.29 g) in an open test tube was heated at 170° C. for 30 minutes. After cooling to room temperature the mixture was diluted with water and extracted with ethyl acetate. The organic phase was washed, dried, and evaporated. Chromatography over silica gel with ethyl acetate gave the title compound, which crystallized from ethyl acetate. Yield, 0.12 g, m.p. 131°-134° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05620974uspto-grants-1997_04