Boron tribromide → HCID 11287639, compound

Temperature

0 °C

To 300 ml of dehydrated dichloromethane solution containing 60.0 g (247 mmol) of 4-bromo-2-cyclopropoxy-1-methoxybenzene obtained in Reference Example 7-(c) was added 300 ml of dichloromethane solution containing 1M boron tribromide under argon atmosphere at −70° C. After completion of the addition, the mixture was gradually raised to 0° C., and stirred at the same temperature for 30 minutes. After completion of the reaction, the reaction mixture was poured into ice-water, and extracted with toluene. The organic layer after separation was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 58.6 g of the title compound as a blue-greenish solid substantially quantitatively.

1. additionAfter completion of the addition
2. customAfter completion of the reaction
3. extractionextracted with toluene
4. customThe organic layer after separation
5. washwas washed with a saturated aqueous solution of sodium chloride
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure

ORD record

ord-63440056bbb84706876a04bf8c1daad5

Source dataset

uspto-grants-2013_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08450319B2