Reaktion #557815

ord-78c50ea9f043450bbc4ac28dbc99e005

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGstirred at 80° C. to 85° C. for 3-4 h
  2. 2
    SonstigeAfter the reaction period
  3. 3
    Sonstigethe reaction mixtures
  4. 4
    Temperaturwas cooled to 25° C. to 30° C.
  5. 5
    Filtrationfiltered
  6. 6
    Waschenwashed with 2 mL of isopropyl alcohol
  7. 7
    SonstigeThe filtrate was collected
  8. 8
    workup.DISTILLATIONdistilled out completely
  9. 9
    Sonstigeto obtain a crude residue

Vorschrift

To a solution of 0.107 g (15.4 mmol) of hydroxylamine hydrochloride in 11 mL of isopropyl alcohol, 1.90 g (22.64 mmol) of sodium bicarbonate was added. The resulting mixture was stirred at 25° C. to 30° C. for 10-15 min. 1.0 g (10.2 mmol) of hexanenitrile was added and stirred at 80° C. to 85° C. for 3-4 h. After the reaction period, the reaction mixtures was cooled to 25° C. to 30° C., filtered and washed with 2 mL of isopropyl alcohol. The filtrate was collected and distilled out completely to obtain a crude residue. The residue with chased with 5 mL of toluene, to yield the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08629277B2uspto-grants-2014_01