Reaktion #581649

ord-e132b16ef53f422793d779137ae29935

Reaktionsbedingungen

Temperatur
25°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux for 6 hours
  2. 2
    WaschenThe organic layer was washed with water (2×) and saturated sodium chloride solution (1×), dried(Na2SO4)
  3. 3
    Filtrationfiltered
  4. 4
    Einengenconcentrated in vacuo
  5. 5
    SonstigeThe residue was triturated with ether
  6. 6
    Filtrationfiltered

Vorschrift

A solution of the product of Example 9E (2.25 g, 8.65 mmol) in dioxane (50 mL) was treated with 1 N HCl solution (60 mL) and the mixture was stirred at reflux for 6 hours, cooled to 25° C., diluted with ethyl acetate and water. The organic layer was washed with water (2×) and saturated sodium chloride solution (1×), dried(Na2SO4), filtered and concentrated in vacuo. The residue was triturated with ether and filtered.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07538105B2uspto-grants-2009_05