Réaction #64717

ord-6029f0ddbc5f49ef962aebcb76173fc8

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températurethe suspension was heated
  2. 2
    Températureunder reflux for 30 minutes
  3. 3
    ConcentrationThe resulting mixture was concentrated under reduced pressure, and water
  4. 4
    workup.ADDITIONwas added to the residue
  5. 5
    ExtractionThe resulting mixture was extracted with ethyl acetate
  6. 6
    Séchagethe extract was dried over anhydrous magnesium sulfate
  7. 7
    ConcentrationAfter concentration under reduced pressure
  8. 8
    Autrethe residue was recrystallized

Mode opératoire

In a mixture of 50 ml of saturated aqueous sodium. hydrogencarbonate solution and 50 ml of methanol was suspended 2.6 g of Compound 2 prepared in Example 1, and the suspension was heated under reflux for 30 minutes. The resulting mixture was concentrated under reduced pressure, and water was added to the residue. The resulting mixture was extracted with ethyl acetate, and the extract was dried over anhydrous magnesium sulfate. After concentration under reduced pressure, the residue was recrystallized to afford 1.23 g of the desired product.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US05413997uspto-grants-1995_05