反应详情

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.

1. temperatureto reflux for 64 h
2. temperatureThe reaction mixture was partially cooled
3. customexcess hydrobromic acid was removed by vacuum distillation (110° C.@2 Torr) until a tan solid residue
4. distillationDistillation
5. filtrationfiltered
6. customdried under a nitrogen stream