Reaction #65848

Reaction equation

2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole

2-(1-Chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole

bromine

→

5-Bromo-2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxol

Solvents

carbon tetrachloride

Conditions

Workup

1. 1
   Temperatureunder reflux
2. 2
   TemperatureAfter cooling
3. 3
   Washit was washed with 10% NaHSO3 solution
4. 4
   Dryingdried over MgSO4
5. 5
   workup.DISTILLATIONdistilled

Procedure

51 g of 2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole from Example 2 or 17 were dissolved in 300 ml of carbon tetrachloride, and 0.5 g of anhydrous FeCl3 was added. 32 g of bromine were then added and the mixture was stirred for 3 hours under reflux. After cooling, it was washed with 10% NaHSO3 solution, dried over MgSO4 and distilled. The yield was 49 g (63% of theory) and the boiling point was 94°-98° C. at 8 mbar.

Source