Reaktion #67459

ord-b54822c1c04740e7b517176eb76e9e43

Lösungsmittel

Reaktionsbedingungen

Temperatur
75°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reagents were evaporated
  2. 2
    Sonstigere-evaporated with chloroform-toluene
  3. 3
    workup.ADDITIONThe residual brown oil was diluted with chloroform (22 mL)

Vorschrift

5′-[(1-Benzo[1,3]dioxol-5-yl-cyclopropanecarbonyl)-amino]-2′-methylbiphenyl-4-sulfonic acid (1.9 g, 4.3 mmol) was dissolved in POCl3 (30 mL) followed by the addition of SOCl2 (3 mL) and DMF (100 μl). The reaction mixture was heated at 70-80° C. for 15 min. The reagents were evaporated and re-evaporated with chloroform-toluene. The residual brown oil was diluted with chloroform (22 mL) and immediately used for sulfonylation. ESI-MS m/z calc. 469.0, found 470.1 (M+1).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524767B2uspto-grants-2013_09