Reaktion #1452191

ord-4fafb7c25e3e441ba38328592ec42f77

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was heated
  2. 2
    Temperaturto reflux for 1.5 hours
  3. 3
    WaschenThe solution was successively washed with water (2×100 mL) and brine (2×100 mL)
  4. 4
    Trocknendried (MgSO4)
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated in vacuo

Vorschrift

To the product of Step 3 (3 g, 9 mmol) was added a 1.0M TBAF solution in THF (9.3 mL, 9.3 mmol). The mixture was heated to reflux for 1.5 hours, cooled to room temperature, and diluted with 500 mL of ethyl acetate. The solution was successively washed with water (2×100 mL) and brine (2×100 mL), dried (MgSO4), filtered, and concentrated in vacuo to provide the desired product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07888464B2uspto-grants-2011_02