Reaktion #58075

ord-7072e1c97cbd4655b956b63c85fe56c9

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationthe precipitated sodium chloride is filtered off
  2. 2
    SonstigeThe reaction mixture is evaporated down
  3. 3
    Temperaturcooled
  4. 4
    FiltrationThe precipitated solid is filtered off
  5. 5
    Waschenwashed with cold ethanol and diethyl ether (5.7 g white solid)

Vorschrift

1.65 g (72 mmol) sodium are dissolved in 80 mL ethanol. 8.89 g (72 mmol) ethyl acetimidate hydrochloride in 160 mL ethanol are added at ambient temperature and the precipitated sodium chloride is filtered off. The filtrate is combined with 6.00 g (40 mmol) 4-methyl-benzoic acid hydrazide and stirred overnight. The reaction mixture is evaporated down and cooled. The precipitated solid is filtered off and washed with cold ethanol and diethyl ether (5.7 g white solid). A further 1.2 g solid are obtained from the filtrate after distillation of the solvents and recrystallisation from ethanol.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07423036B2uspto-grants-2008_09