反应详情

To a mixture of 5-[4-[6-[4-(2-aminoethyl)phenoxy]-1-methyl-1H-benzimidazol-2-ylmethoxy]benzyl]thiazolidine-2,4-dione dihydrochloride (0.3 g), triethylamine (65 mg) and anhydrous N,N-dimethylformamide (5 ml) was added 2,4-difluorophenyl isocyanate (81 mg) and the mixture was stirred at room temperature for 4.5 hours and then allowed to stand for 2 days. The reaction mixture was concentrated and diluted with water and tetrahydrofuran and then extracted with ethyl acetate. The extract was washed with saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate and then concentrated. To the residue was added ethyl acetate and the precipitate was isolated by filtration and washed with ethyl acetate to afford the title compound (0.2 g, mp 161-164° C.).

1. waitto stand for 2 days
2. concentrationThe reaction mixture was concentrated
3. additiondiluted with water and tetrahydrofuran
4. extractionextracted with ethyl acetate
5. washThe extract was washed with saturated aqueous sodium chloride solution
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated
8. additionTo the residue was added ethyl acetate
9. customthe precipitate was isolated by filtration
10. washwashed with ethyl acetate