1H-1,2,4-Triazole → Ethyl 6-[p-[5-(1,2,4-triazol-1-yl)pentyloxy]phenoxy]-2,2-dimethylhexanoate

HRID 329467Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 329467
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][O:7][C:8]1[CH:26]=[CH:25][C:11]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]([CH3:24])([CH3:23])[C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:10][CH:9]=1.[Na].[NH:28]1[CH:32]=[N:31][CH:30]=[N:29]1>CN(C=O)C>[N:28]1([CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][O:7][C:8]2[CH:26]=[CH:25][C:11]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]([CH3:24])([CH3:23])[C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:10][CH:9]=2)[CH:32]=[N:31][CH:30]=[N:29]1

Komponenten

5

Edukt 3

HCID 92571H-1,2,4-TriazoleHCID 5360545SodiumHCID 14851566Ethyl 6-[p-(5-bromopentyloxy)phenoxy]-2,2-dimethylhexanoate

Produkt 1

HCID 14327307Ethyl 6-[p-[5-(1,2,4-triazol-1-yl)pentyloxy]phenoxy]-2,2-dimethylhexanoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of 2.16 g ethyl 6-[p-(5-bromopentyloxy]phenoxy)-2,2-dimethylhexanoate in 10 ml DMF, was added with stirring 0.55 g sodium salt of 1,2,4-triazole at room temperature, and stirring was continued overnight. DMF was distilled off under reduced pressure, the residue was extracted with chloroform, and the extract was washed with water, dried and concentrated. The crude product thus obtained was purified by silica gel column chromatography, affording 1.21 g of ethyl 6-[p-[5-(1,2,4-triazol-1-yl)pentyloxy]phenoxy]-2,2-dimethylhexanoate.

Aufarbeitung

  1. distillationDMF was distilled off under reduced pressure
  2. extractionthe residue was extracted with chloroform
  3. washthe extract was washed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe crude product thus obtained
  7. customwas purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-b822d86399a74df8b5387cc9d1022eb9
Quelldatensatz
uspto-grants-1990_01
Patentnummer
US04891432

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