Reaktion #94749

Reaktionsgleichung

Na2SO4

LiAlH4

1-(3',4'-dimethoxyphenyl)-7-(4'-fluorophenyl)-2-nitro-5-heptanone ethylene ketal

LiAlH4

→

2-Amino-1-(3',4'-dimethoxyphenyl)-7-(4'-fluorophenyl)-5-heptanone ethylene ketal

Lösungsmittel

tetrahydrofuran

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONAfter the addition the reaction mixture
2. 2
   Temperaturwas refluxed gently for 2 hours
3. 3
   FiltrationThe inorganic salts were filtered off
4. 4
   Waschenwashed with ether
5. 5
   ExtraktionThe organic layer was extracted twice with water
6. 6
   Trocknendried over anh MgSO4
7. 7
   Filtrationfiltered
8. 8
   Einengenconcentrated under reduced pressure to 250 ml

Vorschrift

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.

Quelle