Dimethyl Sulfoxide → 272124-01-3

Temperature

100 °C

3-bromophenol (0.582 mol), potassium hydroxide (0.582 mol), methyl sulfoxide (3.2 L) and xylene (0.08 L) were put in a 2-bulb flask equipped with a Dean-Stark azeotropic distillation unit, which has been purged with nitrogen. The reactor was heated to 100° C. and reaction was performed for 48 hours to remove water. The reactor was cooled to 30° C. and 1,2-dibromotetrafluoroethane (0.640 mol) was slowly dropped for 4 hours maintaining the reactor temperature below 30° C. The reaction solution was mixed at 22° C. for 12 hours, and then reaction was performed at 35° C. for 10 hours. After the reaction was completed, the reaction solution was extracted with methylene chloride diluted in water. The obtained product was washed with water for three times and dehydrated with magnesium sulfate. Methylene chloride was removed from the filtrate using a vacuum evaporator. From vacuum distillation, 3-(2-bromotetrafluoroethoxy)bromobenzene was obtained as clear liquid (boiling point: 107 to 110° C.). The yield was 72%.

1. customequipped with a Dean-Stark azeotropic distillation unit, which
2. customhas been purged with nitrogen
3. customreaction
4. customto remove water
5. temperatureThe reactor was cooled to 30° C.
6. temperaturemaintaining the reactor temperature below 30° C
7. additionThe reaction solution was mixed at 22° C. for 12 hours
8. customreaction
9. waitwas performed at 35° C. for 10 hours
10. extractionthe reaction solution was extracted with methylene chloride
11. additiondiluted in water
12. washThe obtained product was washed with water for three times
13. customMethylene chloride was removed from the filtrate
14. customa vacuum evaporator
15. distillationFrom vacuum distillation

ORD record

ord-509771ba8275436589cfaf827adefb21

Source dataset

uspto-grants-2008_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07368514B2