反应详情

To 1 ml of a mixture of 48% aqueous HBr solution and conc. sulfuric acid (2:1 v/v) were added 0.81 g (3.3 mmol) (2,6-bis-trifluoromethyl-phenyl)-methanol and the solution heated to reflux for 6 h. Then the reaction mixture was cooled to rt, diluted with water and extracted with tert-butyl methyl ether. The combined extracts were washed with brine, dried over Na2SO4, filtered and evaporated. Kugelrohr distillation provided 2-bromomethyl-1,3-bis-trifluoromethyl-benzene as colourless oil of b.p. 135-140° C./22 mbar: MS (EI): 307.9 and 305.9 (M+.), 227.1 (((M-Br)+.), 100%).

1. temperaturethe solution heated
2. temperatureto reflux for 6 h
3. extractionextracted with tert-butyl methyl ether
4. washThe combined extracts were washed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customevaporated
8. distillationKugelrohr distillation