Reaktion #671124

ord-9dc17938d4eb4721a7270c640dd99713

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled to room temperature
  2. 2
    Waschenwashed with dichloromethane
  3. 3
    WaschenThe aqueous wash
  4. 4
    Filtrationwas filtered through cotton
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated
  7. 7
    Sonstigedried under vacuum

Vorschrift

A solution of Na2SO3 (400 mg, 3.2 mmol) and NaHCO3 (270 mg, 3.2 mmol) in H2O (10 mL) was treated slowly with a solution of 4-methoxy-3-nitrobenzenesulfonyl chloride (400 mg, 1.6 mmol) in acetone (3 mL), heated to 50° C. for 2 hours, cooled to room temperature, and washed with dichloromethane. The aqueous wash was filtered through cotton, lyophilized, suspended in methanol, filtered, concentrated, and dried under vacuum to provide the desired product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06924304B2uspto-grants-2005_08