Imidazole → Hexaethyldisiloxane

HRID 481802Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 481802
N1[CH:5]=[CH:4]N=C1.[CH2:6]([Si:8](Cl)([CH2:11][CH3:12])[CH2:9][CH3:10])[CH3:7].[OH2:14]>CN(C)C=O>[CH2:6]([Si:8]([O:14][Si:8]([CH2:4][CH3:5])([CH2:9][CH3:10])[CH2:6][CH3:7])([CH2:11][CH3:12])[CH2:9][CH3:10])[CH3:7]

Komponenten

5

Versuchsvorschrift

A solution of 205 (15 mmol) in dimethylformamide (30 mL) is cooled to 0° C. and treated with imidazole (30 mmol) and triethylsilyl chloride (20 mmol). The resultant solution is warmed to room temperature. After 12 h, the reaction mixture is poured into 300 mL of water and extracted with ether (3×40 mL). The ethereal extracts are washed with water (2×25 mL) and saturated aqueous brine (25 mL), dried over magnesium sulfate and concentrated in vacuo. The residue is purified by flash chromatography to afford 206.

Aufarbeitung

  1. extractionextracted with ether (3×40 mL)
  2. washThe ethereal extracts are washed with water (2×25 mL) and saturated aqueous brine (25 mL)
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue is purified by flash chromatography

Quellen und Nachweise

ORD-Eintrag
ord-28682ee2c41649d19b8a2c84c6c050ec
Quelldatensatz
uspto-grants-1998_08
Patentnummer
US05789605

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