Reaktion #732520

ord-5303ce8b359346df922f13f96f7808d8

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwere heated
  2. 2
    Temperaturto reflux temperature for 1 hour
  3. 3
    workup.DISTILLATIONthe mixture was distilled at 220-230° C
  4. 4
    ExtraktionThe distillate was extracted with MTBE
  5. 5
    Waschenthe organic phase washed with water and brine
  6. 6
    Trocknendried (MgSO4)
  7. 7
    Einengenconcentrated in vacuo
  8. 8
    SonstigeThe residue was purified by chromatography

Vorschrift

A mixture of compound (G) (5.00 g), hydrazine hydrate (4.12 g), K2CO3 (7.00 g) and diethylene glycol (16 ml) were heated to reflux temperature for 1 hour. The condenser was exchanged by a distillation device and the mixture was distilled at 220-230° C. The distillate was extracted with MTBE and the organic phase washed with water and brine, dried (MgSO4) and concentrated in vacuo. The residue was purified by chromatography to yield a colorless oil (4.4 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07704942B2uspto-grants-2010_04