Hydrogen Bromide → 3-(3,5-Difluorophenyl)-5-hydroxy-2-(pyridin-3-yl)-1H-inden-1-one

Temperatur

120 °C

To a solution of 3-(3,5-difluorophenyl)-5-methoxy-2-(pyridin-3-yl)-1H-inden-1-one (210 mg, 0.60 mmol) obtained in Step 4 in AcOH (6 mL) was added HBr (3 mL). The mixture was heated to reflux at 120° C. for 16 h. The reaction mixture was cooled to room temperature and neutralized with 3N—NaOH. The resulting solution was extracted with EtOAc (10 mL). The extracts were washed with H2O and brine, dried over MgSO4, and concentrated in vacuo. The residue was purified by recrystallization with CH2Cl2/hexanes to afford the desired product (200 mg, 99%).

1. temperatureThe mixture was heated
2. extractionThe resulting solution was extracted with EtOAc (10 mL)
3. washThe extracts were washed with H2O and brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe residue was purified by recrystallization with CH2Cl2/hexanes

ORD-Eintrag

ord-1ff52a3c09cd4beb9d64f0880d28626c

Quelldatensatz

uspto-grants-2014_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08877747B2