Reaktion #807420

ord-039f15e3488d476f92f8529617b0e6ac

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture heated
  2. 2
    Temperaturto reflux for 1.5 h
  3. 3
    WaschenThe solution was successively washed with water (2×100 mL), brine (2×100 mL)
  4. 4
    Trocknendried (MgSO4)
  5. 5
    Einengenconcentrated in vacuo

Vorschrift

To the product of Step 3 (3 g, 9 mmol) was added a 1.0 M TBAF solution in THF (9.3 mL, 9.3 mmol) and the mixture heated to reflux for 1.5 h, cooled to rt and then diluted with 500 ml of EtOAc. The solution was successively washed with water (2×100 mL), brine (2×100 mL), dried (MgSO4), concentrated in vacuo to provide the title intermediate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07135462B2uspto-grants-2006_11