Reaktion #1348364

ord-2f517c2c51ba44a7a0b6e343ed241729

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe volatile solvents were removed under reduced pressure
  2. 2
    Temperaturthe mixture was heated
  3. 3
    Temperaturto reflux for 10 minutes
  4. 4
    FiltrationThe off white solid was filtered off
  5. 5
    Waschenwashed with water and cold MeOH
  6. 6
    Sonstigedried under high vacuum

Vorschrift

4-Benzyloxy-benzenesulfonyl chloride (7.35 g, 26.0 mmol) was added in small portions to a suspension of 5-amino isophtalic acid dimethyl ester (5.23 g, 25.0 mmol) in DCM (100 ml) and pyridine (10 ml). The resulting clear yellow solution was stirred for 2 hours at room temperature, the volatile solvents were removed under reduced pressure, the solid residue was suspended in MeOH (125 ml) and the mixture was heated to reflux for 10 minutes. The off white solid was filtered off, washed with water and cold MeOH and dried under high vacuum. Yield 10.93 g (96%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08470860B2uspto-grants-2013_06