反应详情

Lithium aluminum hydride, 530 mg. (0.0139 mole), is weighed under nitrogen, transferred to a dry-nitrogen-flushed reaction flask, and suspended in 15 ml. of absolute ether. A solution of 4.15 g. (0.0139 mole) of 2-(α,α,β,β-tetrafluorophenethyl)benzoic acid in 35 ml. of absolute ether is added dropwise. The mixture is stirred at room temperature for 30 minutes and allowed to stand overnight in a nitrogen atmosphere. Hydrolysis is effected by the dropwise addition of 1 ml. of water. The precipitate is removed by filtration, and washed with ether. Evaporation of the dried ethereal filtrate under reduced pressure leaves the product as a white solid, m.p. 80°-81°C. A sample for analysis is sublimed at 70°C. and 0.1 mm.

1. customa dry-nitrogen-
2. customflushed
3. customreaction flask
4. waitto stand overnight in a nitrogen atmosphere
5. customHydrolysis
6. additionis effected by the dropwise addition of 1 ml
7. customThe precipitate is removed by filtration
8. washwashed with ether
9. customEvaporation of the dried ethereal filtrate under reduced pressure