反应详情

2-Chloroisonicotinic acid (5.00 g, 31.7 mmol) was added to thionyl chloride (40 mL), followed by stirring under heating and reflux for 2 hours. The reaction mixture was concentrated under reduced pressure, and the resulting residue was dissolved in dichloromethane (1 mL). The resulting solution was added to a pyridine (16 ml) solution of 2-amino-4-(2-furyl)-5-morpholinothiazole (880 mg, 5.00 mmol) obtained in Step 1 of Example 29, and then N,N-dimethylaminopyridine (48.8 mmol, 0.400 mmol) was added thereto, followed by stirring at room temperature for 1 hour. The reaction mixture was concentrated under reduced pressure, and the resulting residue was purified through silica gel column chromatography (hexane:ethyl acetate=1:3 to ethyl acetate) to afford the entitled Compound 39 (1.05.g, 66%)

1. temperatureunder heating
2. temperaturereflux for 2 hours
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. dissolutionthe resulting residue was dissolved in dichloromethane (1 mL)
5. stirringby stirring at room temperature for 1 hour
6. concentrationThe reaction mixture was concentrated under reduced pressure
7. customthe resulting residue was purified through silica gel column chromatography (hexane:ethyl acetate=1:3 to ethyl acetate)