Reaktion #328674

ord-c8a2086a4f7c400aa766e068b132d21f

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe organic phase was evaporated
  2. 2
    Sonstigeto give a white solid which
  3. 3
    Sonstigeresults
  4. 4
    SonstigeThe mixture was repeatedly recrystallized with ethyl acetate

Vorschrift

Dibenzothiophene (15 g, 79.9 mmol) was dissolved in 1.5 L chloroform. To the solution, bromine (12.76 g, 79.9 mmol) was added dropwise. The reaction mixture was vigorously stirring for 2 days at room temperature and then treated with sodium sulfite water solution. The organic phase was evaporated to give a white solid which has 48% unreacted dibenzothiophene, 50% 2-bromodibenbzothiophene and less 2% 2,8-dibromodibenzothiophene based on GC-MS and HPLC results. The mixture was repeatedly recrystallized with ethyl acetate to get pure 2-bromodibenzothiophene.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08652653B2uspto-grants-2014_02