Reaktion #668098

ord-4d9181fb496a4689bbba6cba446c0511

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeat room temperature
  2. 2
    SonstigeThe methanol was removed in vacuo
  3. 3
    Extraktionthe residue was extracted with methylene chloride (2×50 ml)
  4. 4
    WaschenThe methylene chloride fraction was washed with 1N HCl, H2O, brine
  5. 5
    Trocknendried with anhydrous MgSO4
  6. 6
    Sonstigeevaporated in vacuo

Vorschrift

To a solution of 29 (50 mg) in methanol (5 ml) was added 1 ml solution of K2CO3 and the mixture was stirred for 2 hr. at room temperature. The methanol was removed in vacuo and the residue was extracted with methylene chloride (2×50 ml). The methylene chloride fraction was washed with 1N HCl, H2O, brine, dried with anhydrous MgSO4 and evaporated in vacuo to give 40 mg of 30 (90%) as white crystalline solid which upon TLC analysis (silica, hexane/ethyl acetate, 90:10) showed a single component Rf, 0.4.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05919797uspto-grants-1999_07