Carbon tetrabromide → HCID 19030246, compound

Temperature

0 °C

Next, to a solution comprising 25 g of the previously obtained 4-(3,4-difluorophenyl)benzyl alcohol, 40 g of triphenylphosphine and 80 ml of dichloromethane was added dropwise a solution comprising 64 g of carbon tetrabromide and 35 ml of dichloromethane under stirring at 0° C. After completion of the dropwise addition, the mixture was stirred at the same conditions for one hour, and then raised to room temperature and stirred for one hour to react the materials. After completion of the reaction, the reaction mixture was extracted with hexane, washed with a saturated NaCl aqua, dried and the solvent was removed under reduced pressure, and the residue was purified by recrystallization to obtain 20 g of 4-(3,4-difluorophenyl)benzyl bromide.

1. additionwas added dropwise a solution
2. additionAfter completion of the dropwise addition
3. stirringthe mixture was stirred at the same conditions for one hour
4. temperatureraised to room temperature
5. stirringstirred for one hour
6. customto react the materials
7. customAfter completion of the reaction
8. extractionthe reaction mixture was extracted with hexane
9. washwashed with a saturated NaCl aqua
10. customdried
11. customthe solvent was removed under reduced pressure
12. customthe residue was purified by recrystallization

ORD record

ord-f18d7bcc265241b9a3c381fc60faa840

Source dataset

uspto-grants-1997_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05651919