Boron tribromide → HCID 15125075, compound

To a solution of 4,7-dimethyl-5-methoxyindane (3.5 g) in dichloromethane (30 ml) was added a solution of boron tribromide (5.08 g) in dichloromethane (2 ml) at -78° C. The temperature was raised slowly to room temperature and the mixture was stirred at the same temperature for 1 hour. The mixture was extracted by addition of ice-water (10 ml) and ethyl acetate (50 ml). The organic layer was washed with aqueous sodum bicarbonate, water and saturated saline and dried with anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was recrystallized from hexane to obtain 4,7-dimethyl-5-hydorxyindane (3.2 g) (Compound A-5). The physical properties and NMR spectrum data thereof are shown in Table 1.

1. extractionThe mixture was extracted by addition of ice-water (10 ml) and ethyl acetate (50 ml)
2. washThe organic layer was washed with aqueous sodum bicarbonate, water and saturated saline
3. dry with materialdried with anhydrous magnesium sulfate
4. distillationthe solvent was distilled off under reduced pressure
5. customThe residue was recrystallized from hexane

ORD record

ord-c911f8edc48d4af8adcd54dcce232db3

Source dataset

uspto-grants-1992_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05162571