Reaktion #61078

ord-a57cf86785af40228e02713709f17dc7

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe crude mixture was partitioned between CH2Cl2 and water
  2. 2
    SonstigeThe phases were separated
  3. 3
    Trocknenthe organic layer was dried over anh. Na2SO4
  4. 4
    FiltrationThe solids were filtered
  5. 5
    Sonstigethe solvent evaporated

Vorschrift

To a solution of 6-bromo-2-pyridinamine (1 g, 5.78 mmol) in anh. THF (25 mL), at r.t., under N2, was added 1-chloro-2-isocyanatoethane (1.2 mL, 2.5 eq) and the reaction mixture was stirred at r.t. for 18 hr. The crude mixture was partitioned between CH2Cl2 and water. The phases were separated and the organic layer was dried over anh. Na2SO4. The solids were filtered and the solvent evaporated to give the title compound (1.06 g, 66%) which was used in the next step without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07427630B2uspto-grants-2008_09