Reaktion #62711

ord-0d2c11c9a0654cc6a1af8168abb1e68e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted thrice with 500 ml of ethyl acetate
  2. 2
    WaschenThe extract was washed with water
  3. 3
    Sonstigeafter drying the
  4. 4
    Extraktionextract with anhydrous magnesium sulfate
  5. 5
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure
  6. 6
    SonstigeThe crude crystals obtained
  7. 7
    Sonstigewere recrystallized from benzeneether

Vorschrift

To 250 g of chlorosulfonic acid was added dropwise 50 g of 4-methoxyphenylacetone at 0°-5° C. After stirring the mixture for 4 hours at room temperature, the reaction mixture was poured into 2,500 ml of ice water and extracted thrice with 500 ml of ethyl acetate. The extract was washed with water and after drying the extract with anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure. The crude crystals obtained were recrystallized from benzeneether to provide 32 g of 3-chlorosulfonyl-4-methoxyphenylacetone.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04761500uspto-grants-1988_08