Reaktion #732520
ord-5303ce8b359346df922f13f96f7808d8
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturwere heated
- 2Temperaturto reflux temperature for 1 hour
- 3workup.DISTILLATIONthe mixture was distilled at 220-230° C
- 4ExtraktionThe distillate was extracted with MTBE
- 5Waschenthe organic phase washed with water and brine
- 6Trocknendried (MgSO4)
- 7Einengenconcentrated in vacuo
- 8SonstigeThe 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).