反应详情

1-[3-Morpholin-4-yl-5-(pentafluorosulfanyl)phenyl]ethanone (O2.044; 1.1 g) was dissolved in methanol/THF (20/20 ml) and admixed while stirring with phenyltrimethylammonium tribromide (1.25 g). After stirring at RT for 27 h, 50 ml of 20% citric acid were added and the mixture was stirred for 1 h. After adding DCM (100 ml), the DCM phase was removed, dried and concentrated. The residue was dissolved in acetonitrile (100 ml), and 2 N sulfuric acid (20 ml) was added to the solution. After stirring at RT for 24 h, the mixture was admixed with water and extracted with EA. The EA phase was washed with saturated sodium hydrogencarbonate solution, dried and concentrated. The residue was purified using silica gel (80 g cartridge, n-heptane/EA gradient of 0-60% within 40 min). 866 mg of the title compound were obtained.

1. stirringthe mixture was stirred for 1 h
2. customthe DCM phase was removed
3. customdried
4. concentrationconcentrated
5. dissolutionThe residue was dissolved in acetonitrile (100 ml)
6. addition2 N sulfuric acid (20 ml) was added to the solution
7. stirringAfter stirring at RT for 24 h
8. extractionextracted with EA
9. washThe EA phase was washed with saturated sodium hydrogencarbonate solution
10. customdried
11. concentrationconcentrated
12. customThe residue was purified
13. customsilica gel (80 g cartridge, n-heptane/EA gradient of 0-60% within 40 min)