Reaktion #979299

ord-ae98f0a75b9f4b9ba79e7eab29862792

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGthe mixture was stirred
  2. 2
    Waschenthe organic layer was washed with water
  3. 3
    Trocknendried over magnesium sulfate
  4. 4
    EinengenThe organic layer was concentrated and to the residue
  5. 5
    workup.ADDITIONwere added dichloromethane and diisopropyl ether
  6. 6
    FiltrationThe deposited crystals were collected by filtration

Vorschrift

Compound 67a (82 mg, 0.20 mmol) obtained in Example 67 was dissolved in tetrahydrofuran (1 mL), to the solution was added a 1 mol/L solution (2 mL) of ethyl magnesium bromide in tetrahydrofuran, and the mixture was stirred at 60° C. for 1 hour. To the reaction mixture was added water and the mixture was stirred. Ethyl acetate was added to the mixture and the organic layer was washed with water and dried over magnesium sulfate. The organic layer was concentrated and to the residue were added dichloromethane and diisopropyl ether. The deposited crystals were collected by filtration to obtain the title compound (40 mg, 58%) as a white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07005430B2uspto-grants-2006_02