反应详情

A solution of 3-trifluoromethylbenzyl chloride (25.0g; 0.128 mole) in ether (130 ml) was added dropwise during 50 minutes to magnesium (3.11 g; 0.128 mole) in a three-necked dry flask equipped with stirrer and reflux condenser. The spontaneous reflux was allowed to continue for another half an hour. The solution was cooled and acetone (7.45; 0.128 mole) was added dropwise (8 minutes) and the solution heated to reflux for three hours. After cooling the reaction mixture was poured out on ice (100 ml) and concentrated hydrochloric acid (11 ml). The phases were separated. The organic phase was washed with water, dried (Na2SO4) and evaporated in vacuum. The residual oil was fractioned affording 1-(3-trifluoromethylphenyl)-2-methyl-2-propanol. (B.p. 63°-64° C/1.0 mm Hg, M.p. 55°-56° C recryst. from petroleum ether.) Yield: 73%; 20.3 g.

1. customequipped with stirrer
2. temperaturereflux condenser
3. temperatureThe spontaneous reflux
4. waitto continue for another half an hour
5. temperatureThe solution was cooled
6. temperaturethe solution heated
7. temperatureto reflux for three hours
8. temperatureAfter cooling the reaction mixture
9. customThe phases were separated
10. washThe organic phase was washed with water
11. dry with materialdried (Na2SO4)
12. customevaporated in vacuum