反应详情

温度

0 °C

To a 0° C. solution of 4.64 g of 2-(aminomethyl)pyridine, 13.2 ml of pyridine and 50 ml of methylene chloride is added, dropwise, 15 g of product from Example 53 in 150 ml of methylene chloride. The reaction is stirred at 0° C. for 1 hour followed by 18 hours at room temperature. The reaction is diluted with chloroform, washed with sodium bicarbonate, water and saturated sodium chloride, dried and concentrated in vacuo. The residue is purified by column chromatography (silica gel:75-100% ethyl acetate/hexane) to give 11.0 g of the desired product as colorless prisms.

1. waitfollowed by 18 hours at room temperature
2. washwashed with sodium bicarbonate, water and saturated sodium chloride
3. customdried
4. concentrationconcentrated in vacuo
5. customThe residue is purified by column chromatography (silica gel:75-100% ethyl acetate/hexane)