Реакция #1394

ord-05149c9288364f2583be374274cc2755

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe product crystallized out
  2. 2
    Температураduring slow cooling under agitation
  3. 3
    ФильтрацияAfter 1.5 h agitation in an ice bath the crystals were filtered off
  4. 4
    Промывкаwashed with 150 ml ice water
  5. 5
    Другоеdried in a vacuum at 60° C.
  6. 6
    Сушкаfurther dried in a vacuum desiccator over phosphorus pentaoxide to constant weight

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05723667uspto-grants-1998_03