Reaktion #648276

ord-8136ff04c59840e2b31b05552b340087

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturat reflux for 2 h
  3. 3
    SonstigeA precipitate formed
  4. 4
    Filtrationwas collected by filtration
  5. 5
    Waschenwashed successively with water and ethanol
  6. 6
    Sonstigedried

Vorschrift

A solution of 6 (1.85 g, 5.7 mmol) in a mixture of AcOH—H2O—H2SO4 (8:6:1 v/v, 75 mL) was heated at reflux for 2 h. The reaction mixture was poured into ice water and adjusted to pH 4 with 1M NaOH solution. A precipitate formed and was collected by filtration, washed successively with water and ethanol and then dried to give 7 (1.3 g, 77%) as a light yellow solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08063221B2uspto-grants-2011_11