Reaktion #517613

ord-cd1200984aaf4c78a3063174edcc4d38

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with ethyl acetate
  2. 2
    TrocknenThe combined organic extracts were dried (magnesium sulphate)
  3. 3
    Filtrationfiltered
  4. 4
    Sonstigeevaporated

Vorschrift

A mixture of ethyl 2-(N-ethyl-N-methylsulphonylamino)-4-methylsulphonylbenzoate (11.4 g) and lithium hydroxide monohydrate (1.37 g) in aqueous ethanol (50%) was stirred at room temperature for 19 hours. The mixture was then acidified with conc. hydrochloric acid and extracted with ethyl acetate. The combined organic extracts were dried (magnesium sulphate), filtered and evaporated to yield 2-(N-ethyl-N-methylsulphonylamino)-4-methylsulphonylbenzoic acid as a brown solid (9.48 g), NMR (acetone-d6); 1.15(t,3H), 2.98(s,3H), 3.22(s.3H), 3.85(q,2H), 8.0-8.25(m,3H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06323155B1uspto-grants-2001_11