反应详情

Ethyl 2-phenyl-imidazo[1,2-a]pyridine-8-carboxylate hydrogen bromide (1.96 g, 5.35 m mol), and triethylamine (0.55 g, 5.44 m mol) were added to acetonitrile (20 ml). To this solution was dropwise added a solution of chlorosulfonylisocyanate (ClSO2NCO) (0.8 ml, 9.19 m mol) in acetonitrile (5 ml) at an inner temperature of 0°-20° C. Then, the mixture was allowed to react at room temperature for an hour. After completion of the reaction, the mixture was concentrated under reduced pressure. The resulting concentrate to which water was added was extracted with dichloromethane, and the extract was washed with water, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: chloroform) to give the object compound (1.06 g, yield 67.9%) as crystals. m.p. 87°-89° C.

1. customto react at room temperature for an hour
2. customAfter completion of the reaction
3. concentrationthe mixture was concentrated under reduced pressure
4. concentrationThe resulting concentrate to which water
5. additionwas added
6. extractionwas extracted with dichloromethane
7. washthe extract was washed with water
8. dry with materialdried over anhydrous sodium sulfate
9. concentrationconcentrated under reduced pressure
10. customThe residue was purified by silica gel column chromatography (eluent: chloroform)