Ethyl Acetate → 4-Bromo-2-cyclobutylphenol

Tetra-n-butylammonium tribromide (4.72 g) was added to a solution of 2-cyclobutylphenol (1.21 g) in CH2Cl2 (24.2 mL) at room temperature, and the mixture was stirred at the same temperature overnight. After the reaction mixture was pour into a saturated aqueous sodium sulfite solution, extraction was performed on the mixture using EtOAc, and the extract was washed with water and saturated brine. The organic layer was dried over Na2SO4 and filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (Hex:EtOAc=100:0 to 84:16), whereby 4-bromo-2-cyclobutylphenol (1.85 g) was obtained as a colorless oil.

1. washthe extract was washed with water and saturated brine
2. dry with materialThe organic layer was dried over Na2SO4
3. filtrationfiltered
4. concentrationthe filtrate was concentrated under reduced pressure
5. customThe residue was purified by silica gel column chromatography (Hex:EtOAc=100:0 to 84:16)

ORD-Eintrag

ord-53386a26e45347309ba3293097c0b50a

Quelldatensatz

uspto-grants-2016_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09328118B2