Hydroxyamine hydrochloride → 2-(Hydroxyimino)-3,3-dimethylbutanoic acid

HRID 1379901

반응식

HRID 1379901 반응식
[Na+].[CH3:2][C:3]([CH3:10])([CH3:9])[C:4](=O)[C:5]([O-:7])=[O:6].Cl.[NH2:12][OH:13]>O>[CH3:2][C:3]([CH3:10])([CH3:9])[C:4](=[N:12][OH:13])[C:5]([OH:7])=[O:6]

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 23674764Sodium 3,3-dimethyl-2-oxobutyrate

생성물 1

HCID 713816292-(Hydroxyimino)-3,3-dimethylbutanoic acid수율 81.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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 off under agitation. After 1.5 h agitation in an ice bath the crystals were filtered off, washed with 150 ml ice water and at first pre-dried in a vacuum at 60° C. and then post-dried in a vacuum desiccator over phosphorus pentoxide to constant weight. 117.8 g (yield 81%) trimethylpyruvic acid oxime in the form of colorless crystals were obtained.

후처리

  1. customThe product crystallized out
  2. temperatureduring slow cooling off under agitation
  3. filtrationAfter 1.5 h agitation in an ice bath the crystals were filtered off
  4. washwashed with 150 ml ice water
  5. customat first pre-dried in a vacuum at 60° C.
  6. dry with materialpost-dried in a vacuum desiccator over phosphorus pentoxide to constant weight

출처 및 근거

ORD 기록
ord-aa76e0e4fafb40ec853e5922caca179c
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05672753

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