反应详情

To a suspension of 22.0 g (0.58 mole) of LiAlH4 in 400 ml of dry tetrahydrofuran was added dropwise a solution of 84.8 g (0.2 mole) of 1-(3',4'-dimethoxyphenyl)-7-(4'-fluorophenyl)-2-nitro-5-heptanone ethylene ketal in a minimum amount of dry tetrahydrofuran. After the addition the reaction mixture was refluxed gently for 2 hours. The excess LiAlH4 was decomposed with saturated Na2SO4 solution. The inorganic salts were filtered off and washed with ether. The organic layer was extracted twice with water, dried over anh MgSO4, filtered and concentrated under reduced pressure to 250 ml. This was used in the next step.

1. additionAfter the addition the reaction mixture
2. temperaturewas refluxed gently for 2 hours
3. filtrationThe inorganic salts were filtered off
4. washwashed with ether
5. extractionThe organic layer was extracted twice with water
6. dry with materialdried over anh MgSO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure to 250 ml