Reaktion #49916

ord-f412726c7f4d4c648d141ddadd2a54cf

Lösungsmittel

Reaktionsbedingungen

Temperatur
5°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigefrom separate
  2. 2
    workup.ADDITIONaddition funnels
  3. 3
    Temperaturwhile maintaining the temperature at or below 10° C
  4. 4
    workup.ADDITIONthe addition
  5. 5
    Temperaturthe reaction mixture was warmed to room temperature
  6. 6
    workup.ADDITIONThe reaction was diluted with hexane

Vorschrift

To a stirred suspension of t-butylhydrazine hydrochloride (1 g, 0.008M) in toluene (30 ml) at room temperature was added dropwise a 50% aqueous solution of sodium hydroxide (0.64 g, 0.008M). After 15 minutes, the reaction mixture was cooled to 5° C. and a solution of benzoyl chloride (1.12 g, 0.008M) in toluene (5 ml) and a solution of aqueous 50% sodium hydroxide (0.64 g, 0.008M) were added dropwise simultaneously from separate addition funnels while maintaining the temperature at or below 10° C. Following the addition, the reaction mixture was warmed to room temperature and stirred for 1 hour. The reaction was diluted with hexane and the solid N'-t-butyl-N'-benzoylhydrazine was isolated by filtration.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05424333uspto-grants-1995_06