Reaktion #1970276

ord-20a2a4a7aec34f1fb2e118546033fe66

Reaktionsbedingungen

Temperatur
55°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter a short time, a clear solution was formed
  2. 2
    workup.WAITto stand at room temperature overnight
  3. 3
    workup.STIRRINGstirring
  4. 4
    workup.WAITwas then continued at 60° C. for 6 hours
  5. 5
    workup.STIRRINGthe mixture was stirred with ice-
  6. 6
    Temperaturcooling for 2 h
  7. 7
    FiltrationThe precipitate was filtered off with suction
  8. 8
    Waschenwashed with water
  9. 9
    Trocknendried over phosphorus pentoxide in a desiccator

Vorschrift

11.01 g (50 mmol) of 10.1 and 42.3 g (440 mmol) of ammonium carbonate were suspended in 200 ml of 50% strength ethanol. 4.23 g (65 mmol) of potassium cyanide were added thereto. The mixture was stirred at 50 to 60° C. for 5 hours. After a short time, a clear solution was formed. The mixture was allowed to stand at room temperature overnight and stirring was then continued at 60° C. for 6 hours. Using 6 N HCl, the pH was adjusted to 6.3 and the mixture was stirred with ice-cooling for 2 h. The precipitate was filtered off with suction, washed with water and dried over phosphorus pentoxide in a desiccator. 9.5 g (65%) of 10.2 were obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06759424B2uspto-grants-2004_07