反应详情

A mixture of 5.0 g 2-(aminomethyl)pyridine, 5.02 ml acetic anhydride, 0.847 g 4-dimethylaminopyridine and 35 ml of pyridine is heated at reflux temperature for 23.5 hours. The cooled solution is poured into water and extracted with methylene chloride. The organic layer is washed with saturated sodium chloride, dried and concentrated in vacuo. The residue is purified by column chromatography (silica gel:5% methyl alcohol/ethyl acetate) to give 3.3 g of desired product as a light yellow oil.

1. temperatureis heated
2. temperatureat reflux temperature for 23.5 hours
3. extractionextracted with methylene chloride
4. washThe organic layer is washed with saturated sodium chloride
5. customdried
6. concentrationconcentrated in vacuo
7. customThe residue is purified by column chromatography (silica gel:5% methyl alcohol/ethyl acetate)