Reaktion #1809786

ord-91157b0601a645c98afd01ff642fa4d1

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigedoes not exceed 28° C
  2. 2
    Extraktionextracted with ethyl acetate
  3. 3
    WaschenThe extract is washed with water and hydrochloric acid
  4. 4
    Trocknendried over sodium sulfate
  5. 5
    Einengenconcentrated by evaporation
  6. 6
    SonstigeThe residue is chromatographed through a column of silica gel

Vorschrift

4.5 g of potassium tert-butylate are added in portions to a solution of 5 g of 2-(2-chloroprop-2-enyloxy)phenylsulfonamide such that the temperature does not exceed 28° C. The reaction mixture is stirred for 20 hours at 20°-25° C. and, after addition of ice-water, adjusted to pH 7 by the dropwise addition of 10% hydrochloric acid and extracted with ethyl acetate. The extract is washed with water and hydrochloric acid, dried over sodium sulfate and concentrated by evaporation. The residue is chromatographed through a column of silica gel to give pure 2-allenyloxyphenylsulfonamide of m.p. 94°-95° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04857100uspto-grants-1989_08