Reaktion #1149568

ord-b0b7aff80f8545a1ad69f9e3ae2d2520

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: US06960688B2uspto-grants-2005_11