Reaktion #1352072

ord-010df0db772944dba327f3aadcc759ce

Reaktionsbedingungen

Temperatur
160°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with ethyl acetate
  2. 2
    TrocknenThe extract was dried over anhydrous magnesium sulfate
  3. 3
    Einengenconcentrated in vacuo

Vorschrift

The compound (25.3 g, 154.8 mmol) prepared in Step 1 above was added to polyphosphoric acid (250 g) and then stirred for 1.5 hours at 160° C. The reaction mixture was poured into ice water, neutralized with ammonia solution, and extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate and concentrated in vacuo. The resulting residue was subjected to silica gel column chromatography (eluent: methanol/dichloromethane ={fraction (1/20)}) to give 21.8 g of the titled compound as an oily substance.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06545008B1uspto-grants-2003_04