反应详情

1-[3-Methoxy-5-(pentafluorosulfanyl)phenyl]ethanone (O2.007; 1.63 g) was dissolved in THF (150 ml), and phenyltrimethylammonium tribromide (2.2 g) was added at RT while stirring. After stirring at RT for 2 h, the mixture was admixed with water, neutralized with sodium hydrogencarbonate solution and extracted three times with EA. The alkaline water phase was extracted 3× 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. 1.27 g of the title compound were isolated. LC-MS rt: 1.65 min [M+H]+: 354.9 (met. b)

1. stirringAfter stirring at RT for 2 h
2. extractionextracted three times with EA
3. extractionThe alkaline water phase was extracted 3× with EA
4. dry with materialThe combined organic phases were dried over magnesium sulfate
5. filtrationafter the desiccant had been filtered off
6. customdried under reduced pressure
7. customThe residue was purified by means of preparative HPLC (
8. extractionextracted three times with EA
9. dry with materialThe combined organic phases were dried over magnesium sulfate
10. filtrationafter the desiccant had been filtered off
11. customdried under reduced pressure