Bromine → 2-Bromo-1-[3-bromo-5-(pentafluorosulfanyl)phenyl]ethanone

1-[3-Bromo-5-(pentafluorosulfanyl)phenyl]ethanone (50 mg) was initially charged dissolved in glacial acetic acid (3 ml), and bromine (50 μl of a solution of 475 mg of bromine in 1 ml of glacial acetic acid) was slowly added dropwise. After stirring at RT for 30 min, the mixture was heated to 60° C. for 3 h and then a further 15 μl of the bromine solution were added. After 2 h, the mixture was left to stand overnight, then heated again to 60° C., and a further 10 μl of the bromine solution were added. After 1 h, the mixture was diluted with toluene and dried. The residue was purified by means of preparative HPLC, and the product-containing fractions were combined, freed of the acetonitrile, alkalized with saturated sodium hydrogencarbonate solution and extracted three times with EA. The combined EA phases were dried over magnesium sulfate, filtered and concentrated. 16 mg of the title compound were obtained.

1. temperaturethe mixture was heated to 60° C. for 3 h
2. waitAfter 2 h
3. waitthe mixture was left
4. waitto stand overnight
5. temperatureheated again to 60° C.
6. waitAfter 1 h
7. customdried
8. customThe residue was purified by means of preparative HPLC
9. extractionextracted three times with EA
10. dry with materialThe combined EA phases were dried over magnesium sulfate
11. filtrationfiltered
12. concentrationconcentrated

ORD-Eintrag

ord-c4adb003adf74ec7b9db3a43da3de330

Quelldatensatz

uspto-grants-2013_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08466169B2