Reaktion #1876815

ord-3eaf5a5c4504444dad2bbf538ca8f3b7

Reaktionsbedingungen

Temperatur
-78°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas slowly added dropwise at the same temperature
  2. 2
    Extraktionthe aqueous layer was extracted with ether
  3. 3
    Waschenwashed with saturated aqueous sodium chloride
  4. 4
    Trocknendried over anhydrous magnesium sulfate
  5. 5
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

Vorschrift

Boron tribromide (11.8 g) was slowly added dropwise to dichloromethane (41 mL) cooled to −78° C., and then Compound (e) (6.47 g) dissolved in dichloromethane (60 mL) was slowly added dropwise at the same temperature and the mixture was stirred at room temperature for 2 hours. The reaction mixture was then poured into ice water and the aqueous layer was extracted with ether. The organic layers were combined, washed with saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 3.53 g of Compound (g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07070838B2uspto-grants-2006_07