Alumina → 1-(5-Bromo-2-fluorophenyl)propan-1-one

A mixture of 10 g (42.9 mmol) 1-(5-bromo-2-fluorophenyl)-1-propanol (Example 7A), 8.75 g (85.8 mmol) neutral aluminium oxide and 18.5 g (85.8 mmol) pyridinium chlorochromate in dichloromethane (100 ml) was stirred at room temperature for 4 h. The mixture was then filtered through silica gel (0.06-0.2 mm, 200 g) which was washed thoroughly with dichloromethane (1000 ml). The combined filtrates were washed with brine, dried over sodium sulfate and concentrated under reduced pressure. The crude title compound thus obtained (8.6 g, 87% of th.) was used in the next step without further purification.

1. filtrationThe mixture was then filtered through silica gel (0.06-0.2 mm, 200 g) which
2. washwas washed thoroughly with dichloromethane (1000 ml)
3. washThe combined filtrates were washed with brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated under reduced pressure

ORD record

ord-e353998964954297bf4b8c32c65fa7dd

Source dataset

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09422263B2