反应详情

温度

90 °C

To a stirred solution of 1-piperidin-4-yl-1H-benzimidazole (4.02 g) and 1-(3-chloropropoxy)-4-fluorobenzene (4.16 g) in DMF (50 ml) was added K2CO3 (4.1 g) and KI (0.2 g). The mixture was heated at 90° C. for 2 h, and then allowed to cool to rt. Water (100 ml) was added and the mixture extracted with ethyl acetate (2×80 ml), and the organic layer separated and washed with water. This was further dried and concentrated in vacuo. The free base converted to the hydrochloride salt by action of HCl in ethanol. The solid was recrystallised from ethanol-diethylether to yield 4.7 g of the title compound as colourless crystals. MP. 233-235° C.

1. temperatureto cool to rt
2. extractionthe mixture extracted with ethyl acetate (2×80 ml)
3. customthe organic layer separated
4. washwashed with water
5. customThis was further dried
6. concentrationconcentrated in vacuo
7. customThe solid was recrystallised from ethanol-diethylether