Imidazole → 4-Trimethylsilylethynyl-1-octyn-4-ol trimethylsilyl ether

HRID 848880Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 848880
[CH3:1][Si:2]([C:5]#[C:6][C:7]([OH:15])([CH2:11][CH2:12][CH2:13][CH3:14])[CH2:8][C:9]#[CH:10])([CH3:4])[CH3:3].N1C=CN=C1.Cl[Si:22]([CH3:25])([CH3:24])[CH3:23].CCCCCC>CN(C)C=O>[CH3:23][Si:22]([O:15][C:7]([C:6]#[C:5][Si:2]([CH3:3])([CH3:1])[CH3:4])([CH2:11][CH2:12][CH2:13][CH3:14])[CH2:8][C:9]#[CH:10])([CH3:25])[CH3:24]

Komponenten

6

Edukt 4

HCID 795ImidazoleHCID 6397ChlorotrimethylsilaneHCID 8058HexaneHCID 127861934-Trimethylsilylethynyl-1-octyn-4-ol

Produkt 1

HCID 572330774-Trimethylsilylethynyl-1-octyn-4-ol trimethylsilyl ether

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a stirred mixture of 8.5 g of 4-trimethylsilylethynyl-1-octyn-4-ol and 6.2 g of imidazole in 24 ml of dry dimethylformamide is added, under nitrogen, 5.7 ml of chlorotrimethylsilane, in a slow stream, via a syringe. The mixture is stirred in an ice bath for one hour and then at room temperature overnight. The mixture is poured into hexane, washed with saturated sodium bicarbonate solution, water and then brine and dried over sodium sulfate. The solvents are evaporated to dryness giving 11.1 g of the desired product.

Aufarbeitung

  1. additionis added, under nitrogen
  2. customat room temperature
  3. customovernight
  4. washwashed with saturated sodium bicarbonate solution, water
  5. dry with materialbrine and dried over sodium sulfate
  6. customThe solvents are evaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-36dc43f6fa794f98a157a79fe1e6db8b
Quelldatensatz
uspto-grants-1981_10
Patentnummer
US04297516

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