Reaktion #73984

ord-b972cb7c15c5458b950f4d2b4e5536a5

Reaktionsgleichung

C=C(C)C(=O)Cl
methacryloyl chloride
C[Si](C)(C)CC#CO
trimethylsilyl propyn-1-ol
CCN(CC)CC
Et3N
C=C(C)C(=O)OCC#C[Si](C)(C)C
2-Methyl-acrylic acid 3-trimethylsilanyl-prop-2-ynyl ester

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAny precipitated ammonium salts can be removed by filtration, and volatile components
  2. 2
    Sonstigecan be removed under reduced pressure
  3. 3
    SonstigeThe crude product is then purified by flash chromatography

Vorschrift

A solution of trimethylsilyl propyn-1-ol (1 g, 7.8 mmol) and Et3N (1.4 mL, 10 mmol) in Et2O (10 mL) is cooled to −20° C. and a solution of methacryloyl chloride (0.9 mL, 9.3 mmol) in Et2O (5 mL) is added dropwise over 1 h. The mixture is stirred at this temperature for 30 min, and then allowed to warm to ambient temperature overnight. Any precipitated ammonium salts can be removed by filtration, and volatile components can be removed under reduced pressure. The crude product is then purified by flash chromatography.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08541448B2uspto-grants-2013_09