Reaktion #1394

ord-05149c9288364f2583be374274cc2755

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe product crystallized out
  2. 2
    Temperaturduring slow cooling under agitation
  3. 3
    FiltrationAfter 1.5 h agitation in an ice bath the crystals were filtered off
  4. 4
    Waschenwashed with 150 ml ice water
  5. 5
    Sonstigedried in a vacuum at 60° C.
  6. 6
    Trocknenfurther dried in a vacuum desiccator over phosphorus pentaoxide to constant weight

Vorschrift

163 g (1 mole) 93.5% trimethylpyruvic acid sodium salt and 69.5 g (1 mole) hydroxylamine hydrochloride were dissolved at 40° C. in 450 ml water. The product crystallized out during slow cooling under agitation. After 1.5 h agitation in an ice bath the crystals were filtered off, washed with 150 ml ice water, dried in a vacuum at 60° C., and then further dried in a vacuum desiccator over phosphorus pentaoxide to constant weight. 117.8 g trimethylpyruvic acid oxime (81% yield) in the form of colorless crystals were obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05723667uspto-grants-1998_03