反应详情

温度

100 °C

A mixture of 5-[3-(1-imidazolyl)propyl]-2-methoxypyridine(2.10 g), phosphorus oxychloride (7.44 g) and N,N-dimethylformamide (14.6 g) was stirred at 100° C. for 10 hours. To the reaction mixture was added saturated aqueous sodium acetate and saturated aqueous sodium bicarbonate, and extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried (MgSO4), and concentrated under reduced pressure. The residue was subjected to a silica gel chloromatography. From the fraction eluted with ethyl acetate-methanol (20:1, v/v), 2-chloro-5-[3-(1-imidazolyl)propyl]pyridine (1.28 g, 60%) was obtained. Oily substance.

1. extractionextracted with ethyl acetate
2. washThe ethyl acetate layer was washed with water
3. dry with materialdried (MgSO4)
4. concentrationconcentrated under reduced pressure
5. washFrom the fraction eluted with ethyl acetate-methanol (20:1