Reaktion #157046

ord-afb6c2f3f4194cc7956fbfdf80b47324

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGThe reaction mixture was stirred at RT overnight
  2. 2
    Extraktionextracted with EtOAc
  3. 3
    TrocknenOrganic layer was dried over Na2CO3
  4. 4
    Filtrationfiltered
  5. 5
    Einengenconcentrated

Vorschrift

To a cooled solution (0° C.) of tert-butyl 2-hydroxyethylcarbamate (1.1 eq) in THF, NaH (1.3 eq) was added, stirred for 1 hr, and then 4-chloro-3-nitropyridine (1.0 eq) was added. The reaction mixture was stirred at RT overnight, poured into cold water, and extracted with EtOAc. Organic layer was dried over Na2CO3, filtered, and concentrated to yield tert-butyl 2-(3-nitropyridin-4-yloxy)ethylcarbamate. LCMS (m/z): 284.1 (MH+); LC Rt=2.09 min.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08822497B2uspto-grants-2014_09