Reaktion #67440

ord-92a7e3a9bb8847569ab5f304662d36f1

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeirradiated in the microwave at 140° C. for 10 minutes
  2. 2
    SonstigeVolatiles were removed in vacuo and crude product
  3. 3
    Sonstigewas purified by reverse phase HPLC

Vorschrift

5′-(1-(Benzo[d][1,3]dioxol-5-yl)cyclopropanecarboxamido)-2′-(hydroxymethyl)-N,N-dimethylbiphenyl-4-carboxamide (49 mg, 0.10 mmol) and para-toluenesulfonic acid (38 mg, 0.2 mmol) were dissolved in ethanol (1.0 mL) and irradiated in the microwave at 140° C. for 10 minutes. Volatiles were removed in vacuo and crude product was purified by reverse phase HPLC to afford the pure product (6.4 mg, 13%). ESI-MS m/z calc. 486.2, found 487.5 (M+1)+; retention time 3.17 minutes.

Quelle

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