Reaktion #217795

ord-e96fbc4c8237443aac969a665f78e102

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONAfter completion of addition
  2. 2
    SonstigeAfter completion of reaction
  3. 3
    Sonstigethe whole reaction mixture
  4. 4
    workup.ADDITIONwas diluted with an HPLC mobile phase to 50 mL
  5. 5
    Sonstigeto thereby yield a solution

Vorschrift

Sodium borohydride (170 mg, 4.50 mmol) was added to and dissolved in N,N-dimethylacetamide (1.5 mL) at room temperature, followed by addition of an N,N-dimethylacetamide solution (1.0 mL) of ethyl 1-chloro-2-fluoro-cyclopropane-1-carboxylate (hereinafter the compound will be referred to as “compound (1b)”) (cis/trans=95/5) (500 mg, 3.00 mmol). Cobalt chloride hexahydrate (3.6 mg, 0.015 mmol) was added to the resultant solution at the same temperature. After completion of addition, the resultant mixture was stirred at 40° C. for one hour. After completion of reaction, the whole reaction mixture was diluted with an HPLC mobile phase to 50 mL, to thereby yield a solution containing 381.3 mg (yield: 96%) of the title compound. Yield was determined by means of high performance liquid chromatography (HPLC) (the same shall apply hereinafter).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07381833B2uspto-grants-2008_06