Hydroxyamine hydrochloride → Ethyl 2-(4-(1-(hydroxyimino)propyl)phenoxy)acetate

HRID 68306

Reaktionsgleichung

Reaktionsgleichung von HRID 68306
[C:1]([C:5]1[CH:17]=[CH:16][C:8]([O:9][CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:7][CH:6]=1)(=O)[CH2:2][CH3:3].Cl.[NH2:19][OH:20].C([O-])(=O)C.[Na+]>CO.O>[OH:20][N:19]=[C:1]([C:5]1[CH:17]=[CH:16][C:8]([O:9][CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:7][CH:6]=1)[CH2:2][CH3:3]

Komponenten

6

Edukt 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 24693252Ethyl 2-(4-propionylphenoxy)acetate

Produkt 1

HCID 86699619Ethyl 2-(4-(1-(hydroxyimino)propyl)phenoxy)acetateAusbeute 76,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution of the product of step 1 (49 g, 0.2076 moles) in methanol (343 ml), hydroxylamine hydrochloride (28.6 g, 0.4152 moles) and a solution of sodium acetate (34 g, 0.4152 moles) in water (147 ml) were added and the reaction mixture was refluxed for 1 hour. The solvents were evaporated under reduced pressure. The residue was dissolved in water and extracted with ethyl acetate. The combined ethyl acetate extract was washed with water & brine, dried over sodium sulphate and evapourated under reduced pressure to yield 40 gm (76%) of product as solid.

Aufarbeitung

  1. temperaturethe reaction mixture was refluxed for 1 hour
  2. customThe solvents were evaporated under reduced pressure
  3. dissolutionThe residue was dissolved in water
  4. extractionextracted with ethyl acetate
  5. extractionThe combined ethyl acetate extract
  6. washwas washed with water & brine
  7. dry with materialdried over sodium sulphate

Quellen und Nachweise

ORD-Eintrag
ord-bac0e94301054ed7a1dca8242b51a003
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08822414B2

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