Reaktion #2388227

ord-0c0bbef837e04fefafc2345bac8a9afd

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter 24 hours volatile material was removed by evaporation
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
  3. 3
    Waschenwashed with water
  4. 4
    workup.ADDITIONthe organic layer was poured onto a Varian Chem Elut column
  5. 5
    WaschenElution with ethyl acetate

Vorschrift

Dimethylamine (0.17 ml of a 40% solution in water) was added to a solution of (R)-N-{2-chloro-4-[4-(2-chloroacetylamino)phenylsulphanyl}phenyl -2-acetoxy-2-methyl-3,3,3-trifluoropropanamide (Method 19) (0.25 g) in acetone (1.5 ml). After 24 hours volatile material was removed by evaporation and the residue was dissolved in ethyl acetate, washed with water, and the organic layer was poured onto a Varian Chem Elut column. Elution with ethyl acetate gave the title compound (0.25 g) as a foam. NMR: 1.6 (s, 3H), 3.1 (s, 2H), 3.3 (s, 6H), 7.2 (d, 1H), 7.3 (s, 1H), 7.4 (d, 2H), 7.7 (m, 3H), 7.9 (d, 1H), 9.7 (s, 1H), 9.9 (s, 1H); MS (ESP−): 474.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06498275B1uspto-grants-2002_12