Réaction #2380305

ord-d7869253a49043a1b675031e29f82c8d

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autrewas reacted at 160° C. for 1.5 hours
  2. 2
    Extractionextracted from ethyl acetate
  3. 3
    SéchageThe extract was dried over anhydrous magnesium sulfate
  4. 4
    Concentrationconcentrated under a reduced pressure
  5. 5
    AutreThe residue thus obtained

Mode opératoire

8.43 g of the compound(51.6 mM) prepared in Step 1 above was added to 84.36 g of polyphosporic acid, which was reacted at 160° C. for 1.5 hours with stirring. The reaction solution was poured into ice water, neutralized with ammonia water, and extracted from ethyl acetate. The extract was dried over anhydrous magnesium sulfate and concentrated under a reduced pressure. The residue thus obtained was subjected to silica gel column chromatography using a mixed solvent of methanol:dichloromethane (1:20 (v/v)) as a developing solvent to give 6.48 g of the title compound as oily substance.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US05686458uspto-grants-1997_11