Reaktion #580576

Reaktionsgleichung

(6-o-tolylpyridin-3-yl)methanol

hydrobromic acid

→

product

Ausbeute 95.0%

5-(Bromomethyl)-2-o-tolylpyridine hydrobromide

Ausbeute 95.0%

Reaktionsbedingungen

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