Reaktion #46918

ord-26b8734ec46f438d851b80c723a17934

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling the mixture
  2. 2
    Einengenwas concentrated under reduced pressure
  3. 3
    workup.ADDITIONEther (50 mL) was added to the residue
  4. 4
    Sonstigethe precipitate was isolated by filtration
  5. 5
    WaschenThe pale yellow solid was washed with ether
  6. 6
    Sonstigedried

Vorschrift

A mixture of Example 1A (3.3 g, 10.1 mmol) and 4-aminobenzenesulfonamide (1.74 g, 10.1 mmol) in glacial acetic acid (75 mL) was heated to 100° C. for 48 hours. After cooling the mixture was concentrated under reduced pressure. Ether (50 mL) was added to the residue and the precipitate was isolated by filtration. The pale yellow solid was washed with ether and dried. 1H NMR (CDCl3) δ ppm 1.32 (3H), 2.20 (3H), 3.50 (2H), 4.27 (2H), 6.85 (1H), 7.30-7.90 (8H); MS (ESI) m/z m/z 462/464.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07741364B2uspto-grants-2010_06