Reaktion #3882

ord-37b5bfcf3c62463e96183b6c7a43b894

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenAfter ca. 5 min. at room temperature the solution was concentrated to about half volume
  2. 2
    workup.ADDITIONdiluted with ethyl acetate
  3. 3
    Waschenby washing with two portions of 0.5M potassium bisulfate
  4. 4
    Trocknendried over magnesium sulfate
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated in vacuo
  7. 7
    SonstigeThe crude product was recrystallized

Vorschrift

The title compound of Example 8 (32.0 g, 0.1 mole) was dissolved in 200 ml of methanol to which was added 200 ml of 2M potassium hydroxide. After ca. 5 min. at room temperature the solution was concentrated to about half volume and diluted with ethyl acetate. The solution was neutralized by washing with two portions of 0.5M potassium bisulfate, and then dried over magnesium sulfate, filtered, and concentrated in vacuo. The crude product was recrystallized to give the title compound, which was used in subsequent reactions without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04722922uspto-grants-1988_02