反应详情

温度

-5 °C

1-[3-Amino-5-(pentafluorosulfanyl)phenyl]ethanone (O4.050; 3.00 g) was dissolved in 35% aqueous sulfuric acid (25 ml) while heating. The solution was cooled to −5° C. and a solution of sodium nitrite (780 mg) in 15 ml of water was added dropwise within 10 min. After 40 min at −5° C., the cooling bath was removed and the mixture was heated to 100° C. for 2 h. After cooling, the mixture was extracted twice with EA. The combined EA phases were washed with saturated sodium hydrogencarbonate solution, dried, filtered and concentrated. The residue was purified using silica gel (80 g cartridge, n-heptane/MtB ether gradient of 0-100% within 40 min). 1.62 g of the title compound were obtained.

1. temperaturewhile heating
2. customthe cooling bath was removed
3. temperaturethe mixture was heated to 100° C. for 2 h
4. temperatureAfter cooling
5. extractionthe mixture was extracted twice with EA
6. washThe combined EA phases were washed with saturated sodium hydrogencarbonate solution
7. customdried
8. filtrationfiltered
9. concentrationconcentrated
10. customThe residue was purified
11. customsilica gel (80 g cartridge, n-heptane/MtB ether gradient of 0-100% within 40 min)