Reaktion #1756718

ord-5ff9a623ad664f6198fef4ec9557be5d

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeTFA was removed under vacuum
  2. 2
    workup.WAITGradient conditions: 25% solvent B/75% solvent A to 95% solvent B/5% solvent B over 6 minutes

Vorschrift

C2HF3O2 (1b): TFA (10 mL, 129.8 mmol) was added to intermediate (1a) (5.0 g, 10.2 mmol). The mixture was stirred at 80° C. for 2 hours. TFA was removed under vacuum and the crude intermediate (1b), as a TFA salt, was used in the next step (5.6 g). Anal. HPLC: retention time=3.4 minutes. Gradient conditions: 25% solvent B/75% solvent A to 95% solvent B/5% solvent B over 6 minutes. MS m/z: [M+H]+ calcd for C21H22ClN3O3S, 432.11; found 432.2.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07989484B2uspto-grants-2011_08