Reaktion #60253

ord-53503719160343d8abc4a2bd283b044f

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed with water
  2. 2
    TrocknenThe organic layer is dried over MgSO4
  3. 3
    Filtrationfiltered
  4. 4
    Einengenconcentrated
  5. 5
    Sonstigepurified by flash chromatography (2% MeOH in CH2Cl2)

Vorschrift

To a solution of (2-bromo-ethoxy)-carbamic acid tert-butyl ester (252 mg, 1.05 mmol) in DMF (2 mL) at room temperature is added morpholine (0.14 mL, 1.6 mmol). The reaction mixture is stirred for 7 hours at 50° C. The reaction mixture is diluted with EtOAc, and washed with water. The organic layer is dried over MgSO4, filtered, concentrated, and purified by flash chromatography (2% MeOH in CH2Cl2) to give the desired product (118 mg, 46%): MS APCI (+) m/z 247 detected.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07425637B2uspto-grants-2008_09