Reaktion #96158

ord-65599b480f224c92bde4e20f790dccd9

Reaktionsgleichung

Cc1ccccc1B(c1ccccc1C)c1ccccc1C.N
tri-o-tolylborane ammonia
[C-]#N.[Na+]
sodium cyanide
[C-]#N.[Na+]
sodium cyanide
Cc1ccccc1B(c1ccccc1C)c1ccccc1C
tri-o-tolylborane

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATIONwas distilled from the solution at atmospheric pressure
  2. 2
    workup.ADDITIONAn additional 100 ml of distilled water was then added to the distillation flask and 100 ml of dilute ammonium hydroxide
  3. 3
    workup.DISTILLATIONdistilled
  4. 4
    Sonstigewas then combined at room temperature under agitation with a solution
  5. 5
    Sonstigeprepared
  6. 6
    SonstigeThe gray precipitate which formed as the solutions
  7. 7
    Filtrationwere combined was collected by vacuum filtration
  8. 8
    Waschenwashed with 100 ml of concentrated ammonium hydroxide
  9. 9
    Sonstigedried under vacuum at 50° C. for 4 hours
  10. 10
    SonstigeThe results of the analysis

Vorschrift

A sodium cyanide adduct of tri-o-tolylborane was prepared by dissolving 2.1731 g of the tri-o-tolylborane ammonia adduct [(o-CH3C6H4)3BNH3 ] and 0.3495 g of sodium cyanide in 100 ml of distilled water, following which approximately 80 ml of ammonium hydroxide was distilled from the solution at atmospheric pressure. An additional 100 ml of distilled water was then added to the distillation flask and 100 ml of dilute ammonium hydroxide distilled therefrom. This resultant solution was then combined at room temperature under agitation with a solution prepared by dissolving 0.8608 g of nickel chloride hexahydrate in 50 ml of concentrated ammonium hydroxide (28-30% NH3). The gray precipitate which formed as the solutions were combined was collected by vacuum filtration, washed with 100 ml of concentrated ammonium hydroxide and then dried under vacuum at 50° C. for 4 hours. The product which weighed 2.4069 g was submitted for elemental analysis. The results of the analysis and the calculated formula for the complex Ni[NH3 ]4 [(NC)B(C6H4CH3 -o)3 ]2 are set forth below.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04347193uspto-grants-1982_08