Reaktion #94210

ord-2122063c84c848c19820fb2b2aa12265

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto evaporate
  2. 2
    workup.DISSOLUTIONthe residue is dissolved in water
  3. 3
    Temperaturis heated within a short time on the water-bath
  4. 4
    Filtrationis filtered
  5. 5
    workup.ADDITIONafter the addition of active charcoal
  6. 6
    Filtrationthe precipitate is filtered off with suction
  7. 7
    Waschenis washed with water
  8. 8
    Sonstigeis in the range of from 205° to 208° C.
  9. 9
    Sonstigeafter recrystallization
  10. 10
    workup.ADDITIONfrom a mixture of acetone and water it
  11. 11
    Sonstigeis 216° to 218° C.

Vorschrift

99.6 Grams of 5-chloro-6-chlorosulfonyl-1-indanone are introduced portionwise into 700 ml of liquid ammonia. The solvent is allowed to evaporate and the residue is dissolved in water, is heated within a short time on the water-bath and is filtered after the addition of active charcoal. The solution is acidified with hydrochloric acid to a pH of 2, the precipitate is filtered off with suction and is washed with water. The melting point of 5-chloro-6-sulfamoyl-1-indanone is in the range of from 205° to 208° C., and after recrystallization from a mixture of acetone and water it is 216° to 218° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04129656uspto-grants-1978_12