Reaktion #43464

ord-d88c9ab17aa946a0954bc72cc2376f62

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigequenched with water
  2. 2
    ExtraktionThe product was extracted with CH2Cl2
  3. 3
    Waschenthe organics were washed with saturated aqueous NaHCO3
  4. 4
    Trocknendried over Na2SO4
  5. 5
    Einengenconcentrated
  6. 6
    SonstigePurification by silica gel chromatography (5% EtOAc in hexanes)

Vorschrift

To a stirred solution of compound 1G (1.9 g, 15.1 mmol) in CH2Cl2 (10 mL) at 0° C. under nitrogen were added Et3N (3.1 mL, 22.2 mmol) and benzoyl chloride (2.33 g, 16.6 mmol). The reaction was stirred at 0° C. for 60 min and RT for 30 min, then quenched with water. The product was extracted with CH2Cl2, the organics were washed with saturated aqueous NaHCO3, dried over Na2SO4, and concentrated. Purification by silica gel chromatography (5% EtOAc in hexanes) provide the title compound (3 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07732480B2uspto-grants-2010_06