反应详情

温度

15 °C

A solution of allyl-(5,6-dichloro-pyridin-3-yl)-(2,2-dimethoxy-ethyl)-amine (57.2 g) in tetrahydrofuran (443 g) was cooled to 10° C. A solution of concentrated hydrochloric acid (136 g) in water (114 g) was slowly added, maintaining the temperature below 20° C. The reaction was then stirred at 15° C. for about 4 hours. Then dichloromethane (570 g) and water (430 g) were added and the layers separated. The organic layer was washed with 5% aqueous sodium bicarbonate (453 g), and then washed twice with water (430 g). The organic layer was concentrated and the residue dissolved in dichloromethane (580 g).

1. temperaturemaintaining the temperature below 20° C
2. customthe layers separated
3. washThe organic layer was washed with 5% aqueous sodium bicarbonate (453 g)
4. washwashed twice with water (430 g)
5. concentrationThe organic layer was concentrated
6. dissolutionthe residue dissolved in dichloromethane (580 g)