Reaktion #668845

ord-acded5627ff04c47b809c9982851e0f7

Lösungsmittel

Reaktionsbedingungen

Temperatur
35°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe solution is concentrated under reduced pressure
  2. 2
    Waschenthe mixture is washed successively with dilute hydrochloric acid, saturated NaHCO3 solution and saturated NaCl solution
  3. 3
    TrocknenAfter drying over MgSO4
  4. 4
    Einengenthe organic phase is concentrated

Vorschrift

115 g of N-tert.-butyl-2-methoxycarbonyl-5-nitro-benzenesulfonamide (Example c) in 1500 ml of methanol are gassed with about 200 g of dimethylamine. The mixture is stirred at about 35° C. for one week. The solution is concentrated under reduced pressure, the residue is taken up in ethyl acetate and the mixture is washed successively with dilute hydrochloric acid, saturated NaHCO3 solution and saturated NaCl solution. After drying over MgSO4, the organic phase is concentrated. 92 g of N-tert.-butyl-2-dimethylaminocarbonyl-5-nitro-benzensulfonamide are obtained: m.p.: 138-141° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05922646uspto-grants-1999_07