反应详情

To a suspension of 16.5 g (0.43 mole) of LiAlH4 in 500 ml of dry tetrahydrofuran was added dropwise a solution of 65 g (0.14 mole) of 1-(3',4'-dimethoxyphenyl)-7-(4'-chlorophenyl)-2-nitroheptan-5-one ethylene ketal in a minimum amount of dry tetrahydrofuran. After the addition the reaction mixture was refluxed gently for 2 hrs. The excess LiAlH4 was decomposed with saturated MgSO4 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 hrs
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