Sodium Hydroxide → 1,2,2,6,6-Pentamethyl-piperidin-4-one oxime

HRID 1070699

Reaktionsgleichung

Reaktionsgleichung von HRID 1070699
I.[CH3:2][N:3]1[C:8]([CH3:10])([CH3:9])[CH2:7][C:6](=O)[CH2:5][C:4]1([CH3:13])[CH3:12].Cl.[NH2:15][OH:16].[OH-].[Na+]>O>[CH3:2][N:3]1[C:8]([CH3:10])([CH3:9])[CH2:7][C:6](=[N:15][OH:16])[CH2:5][C:4]1([CH3:13])[CH3:12]

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 223975731,2,2,6,6-Pentamethyl-4-piperidone hydroiodide

Produkt 1

HCID 2419501,2,2,6,6-Pentamethyl-piperidin-4-one oximeAusbeute 83,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

A suspension of 1,2,2,6,6-pentamethyl-4-piperidone hydroiodide (3 g, 10.1 mmol) and hydroxylamine hydrochloride (980 mg, 14 mmol) in water (6 ml) was stirred at RT for 15 minutes. Solid NaOH was added until basic pH and thickening of the suspension. Water (3 ml) was added and stirring at RT was continued overnight. The suspension was filtered and the solid washed with water (few ml) and dried. The solid was then dissolved in Et2O, the solution was dried (MgSO4) and concentrated to give after drying pure title compound (1.55 g, 8.41 mmol, yield 83.3%) as white crystals.

Aufarbeitung

  1. stirringstirring at RT
  2. waitwas continued overnight
  3. filtrationThe suspension was filtered
  4. washthe solid washed with water (few ml)
  5. customdried
  6. dissolutionThe solid was then dissolved in Et2O
  7. dry with materialthe solution was dried (MgSO4)
  8. concentrationconcentrated
  9. customto give

Quellen und Nachweise

ORD-Eintrag
ord-20f3f91506e544d7a8f2cfe8052b4ca4
Quelldatensatz
uspto-grants-2005_06
Patentnummer
US06903117B2

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