Reaktion #2307437

ord-aa7d8e97bd8240d68dc26c457c9eb7ff

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto reflux for 64 h
  2. 2
    TemperaturThe reaction mixture was partially cooled
  3. 3
    Sonstigeexcess hydrobromic acid was removed by vacuum distillation (110° C. @ 2 Torr) until a tan solid residue
  4. 4
    workup.DISTILLATIONDistillation
  5. 5
    Filtrationfiltered
  6. 6
    Sonstigedried under a nitrogen stream

Vorschrift

A solution of 4.49 g (22.5 mmol) of (6-o-tolylpyridin-3-yl)methanol in 75 mL of 48% hydrobromic acid was heated to reflux for 64 h. The reaction mixture was partially cooled and excess hydrobromic acid was removed by vacuum distillation (110° C. @ 2 Torr) until a tan solid residue remained in the flask. Distillation was carried out using a large KOH pellet trap placed between the distillation apparatus and the vacuum pump. The solid residue was slurried in diethyl ether, filtered and dried under a nitrogen stream to give 7.38 g of product, 95% yield.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07417028B2uspto-grants-2008_08