反应详情

To a solution of ethyl 3-[4-(6-methoxy-1-methyl-1H-benzimidazol-2-ylmethoxy)phenyl]-2-methylthiopropionate (2.0 g) in tetrahydrofuran (25 ml) were added successively potassium hydroxide monohydrate (0.42g), and dimethylformamide (5 ml). The mixture was stirred at room temperature for 2 hours. After addition of potassium hydroxide (0.42 g) and water (5 ml) the mixture was stirred at room temperature for 20 minutes. And then after addition of dimethylformamide (5 ml) the mixture was further stirred at room temperature for 1 hour and allowed to stand over night. To the reaction mixture was further added potassium hydroxide (0.42 g), water (5 ml) and dimethylformamide (5 ml) and the the mixture was stirred at 75° C. for 8 hours. The reaction mixture was poured into 1N hydrochloric acid (800 ml), stirred for 30 minutes and filtrated to give crystals. The crystals were washed successively with water, acetone and ethyl acetate and dried under reduced pressure to afford the title compound (1.27 g, mp 201-206° C.).

1. stirringwas stirred at room temperature for 20 minutes
2. stirringwas further stirred at room temperature for 1 hour
3. waitto stand over night
4. stirringthe the mixture was stirred at 75° C. for 8 hours
5. stirringstirred for 30 minutes
6. filtrationfiltrated
7. customto give crystals
8. washThe crystals were washed successively with water, acetone and ethyl acetate
9. customdried under reduced pressure