Water → 2-(4-Chlorophenoxy)-4,4-dimethyl-1-pyridin-3-yl-1-penten-3-one

HRID 443844

Reaktionsgleichung

Reaktionsgleichung von HRID 443844
O.[OH-].[Na+].[Cl:4][C:5]1[CH:18]=[CH:17][C:8]([O:9][CH2:10][C:11](=[O:16])[C:12]([CH3:15])([CH3:14])[CH3:13])=[CH:7][CH:6]=1.[N:19]1[CH:24]=[CH:23][CH:22]=[C:21]([CH:25]=O)[CH:20]=1>CO>[Cl:4][C:5]1[CH:18]=[CH:17][C:8]([O:9][C:10]([C:11](=[O:16])[C:12]([CH3:14])([CH3:15])[CH3:13])=[CH:25][C:21]2[CH:20]=[N:19][CH:24]=[CH:23][CH:22]=2)=[CH:7][CH:6]=1

Komponenten

6

Versuchsvorschrift

100 ml of water, followed by 28 ml of 10% strength aqueous sodium hydroxide solution, were added to a stirred solution of 22.6 g (0.1 mol) of 1-(4-chlorophenoxy)-3,3-dimethyl-butan-2-one and 21.4 g (0.2 mol) of 3-pyridinealdehyde in 500 ml of methanol. The solution was subsequently stirred at room temperature for 4 days, the methanol was removed in vacuo and the aqueous residue was taken up in ether. The aqueous phase was separated off, the organic phase was extracted three times with 1 N hydrochloric acid and the hydrochloric acid extracts were neutralized with solid sodium bicarbonate and extracted three times with ethyl acetate. 22.8 g (72% of theory) Of 2-(4-chlorophenoxy)-4,4-dimethyl-1-pyridin-3-yl-1-penten-3-one of melting point 74°-76° C. were obtained from the ethyl acetate phase.

Aufarbeitung

  1. customthe methanol was removed in vacuo
  2. customThe aqueous phase was separated off
  3. extractionthe organic phase was extracted three times with 1 N hydrochloric acid
  4. extractionextracted three times with ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-57ed26b9f8c64311ad3785c3d0600b05
Quelldatensatz
uspto-grants-1981_04
Patentnummer
US04262000

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