Reaktion #65460

Reaktionsgleichung

lithium aluminium hydride

6-hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylcarbonyl}-1,4-benzodioxin

→

6-Hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin -1-ylmethyl}-1,4-benzodioxin

Ausbeute 85.0%

Lösungsmittel

diethyl ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturUnder a nitrogen atmosphere, heat
2. 2
   TemperaturAfter cooling
3. 3
   Sonstigehydrolysis, removal of the insoluble mineral compounds
4. 4
   Filtrationby filtration
5. 5
   Trocknendrying over magnesium sulfate
6. 6
   Sonstigethe compound obtained
7. 7
   Sonstigeis purified by chromatography on a column of silica (eluant:petroleum ether/ethyl acetate, 40:60)

Vorschrift

Under a nitrogen atmosphere, heat at reflux for 3 hours, in the presence of 5 mmol of lithium aluminium hydride, a solution of 2 mmol of 6-hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylcarbonyl}-1,4-benzodioxin in 35 cm3 of diethyl ether. After cooling, hydrolysis, removal of the insoluble mineral compounds by filtration and drying over magnesium sulfate, the compound obtained is purified by chromatography on a column of silica (eluant:petroleum ether/ethyl acetate, 40:60). 6-Hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin -1-ylmethyl}-1,4-benzodioxin is thereby obtained in a yield of 85%.

Quelle