反应 #1394

ord-05149c9288364f2583be374274cc2755

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The product crystallized out
  2. 2
    温度during slow cooling under agitation
  3. 3
    过滤After 1.5 h agitation in an ice bath the crystals were filtered off
  4. 4
    洗涤washed with 150 ml ice water
  5. 5
    其他dried in a vacuum at 60° C.
  6. 6
    干燥further dried in a vacuum desiccator over phosphorus pentaoxide to constant weight

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05723667uspto-grants-1998_03