Reaktion #304359

ord-83b66e76e2d844a58e71bd9fb500c207

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.WAITwas continued for a further 48 h
  2. 2
    SonstigeThe precipitated solid was collected
  3. 3
    Waschenwashed with DMSO, H2O, i-PrOH, and EtOAc
  4. 4
    Sonstigevacuum-dried

Vorschrift

A solution of KH2PO4 (81 mg, 0.59 mmol) in H2O (3 mL) was added to a solution of 7-iodofuro[3,2-c]pyridine-2-carbaldehyde (578 mg, 2.12 mmol) in DMSO (16 mL). The stirred mixture was treated carefully with a solution of NaClO2 (335 mg, 2.96 mmol) in H2O (5 mL). After 16 h, more KH2PO4 (81 mg, 0.59 mmol) in H2O (3 mL) and NaClO2 (335 mg, 2.96 mmol) in H2O (5 mL) were added, then stirring was continued for a further 48 h. The precipitated solid was collected, washed with DMSO, H2O, i-PrOH, and EtOAc, and vacuum-dried to furnish the title compound: m/z (ES+)=289.9 [M+H]+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08193359B2uspto-grants-2012_06