反应详情

温度

0 °C

To a 0° C. solution of 3.0 g of product from Example 87 is added 50 ml of methylene chloride, 0.829 g of 2-(aminomethyl)pyridine and 2.31 g of pyridine. The reaction is stirred at 0° C. for 3 hours; followed by 20 hours at room temperature. The mixture is poured into chloroform and saturated sodium bicarbonate. The aqueous layer is extracted with chloroform and the combined chloroform layers are washed with saturated sodium chloride, dried and concentrated in vacuo. The residue is purified by column chromatography (silica gel: 75% ethyl acetate/hexane) to give 2.90 g of the desired product as a colorless solid.

1. waitfollowed by 20 hours at room temperature
2. extractionThe aqueous layer is extracted with chloroform
3. washthe combined chloroform layers are washed with saturated sodium chloride
4. customdried
5. concentrationconcentrated in vacuo
6. customThe residue is purified by column chromatography (silica gel: 75% ethyl acetate/hexane)