反应详情

温度

25 °C

70% nitric acid (1.2 ml) was added to acetic anhydride (5 ml) while stirring and maintaining the temperature between 20-30° C. by external cooling. The mixture was cooled to −5° C. while stirring, followed by the addition of 1 gram of N-[5-(2-hydroxy-ethyl)-4-methyl-thiazol-2-yl]-nicotinamide. After 30 minutes at −5° C. the mixture was heated to 10° C. and stirred for one additional hour. The resulting mixture was poured into ice-water and stirred for 1 hour. Aliquots of NaHCO3 were added until CO2 evolution ceased. The orange-yellow water solution was extracted with three portions of 15 ml ethyl acetate. The combined extracts were dried over sodium sulfate and concentrated by evaporation.

1. temperatureThe mixture was cooled to −5° C.
2. stirringwhile stirring
3. temperatureAfter 30 minutes at −5° C. the mixture was heated to 10° C.
4. stirringstirred for one additional hour
5. stirringstirred for 1 hour
6. extractionThe orange-yellow water solution was extracted with three portions of 15 ml ethyl acetate
7. dry with materialThe combined extracts were dried over sodium sulfate
8. concentrationconcentrated by evaporation