反应详情

温度

80 °C

N-[3-(2-Bromoacetyl)-5-(pentafluorosulfanyl)phenyl]-2,2,2-trifluoro-N-methylacetamide (O1.075; 1.2 g) was admixed with water (15 ml), and concentrated sulfuric acid (15 ml) was added dropwise while stirring and with ice cooling. The mixture was heated to 80° C. and stirred at this temperature for 7 h. After cooling, the reaction mixture was added slowly to a mixture of 10 N sodium hydroxide solution and EA, and the aqueous phase was extracted five times with EA. The combined organic phases were dried over magnesium sulfate and, after the desiccant had been filtered off, dried under reduced pressure. The residue was purified by means of preparative HPLC (met. A). The product fractions, each of them clean, were combined, freed of the acetonitrile under reduced pressure, neutralized with sodium hydrogencarbonate and extracted three times with EA. The combined organic phases were dried over magnesium sulfate and, after the desiccant had been filtered off, dried under reduced pressure. 420 mg of the title compound were isolated.

1. additionwas added dropwise
2. stirringstirred at this temperature for 7 h
3. temperatureAfter cooling
4. extractionthe aqueous phase was extracted five times with EA
5. dry with materialThe combined organic phases were dried over magnesium sulfate
6. filtrationafter the desiccant had been filtered off
7. customdried under reduced pressure
8. customThe residue was purified by means of preparative HPLC (
9. extractionextracted three times with EA
10. dry with materialThe combined organic phases were dried over magnesium sulfate
11. filtrationafter the desiccant had been filtered off
12. customdried under reduced pressure