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

HRID 1756038Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1756038
[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH:7][C:8]1[CH:40]=[CH:39][C:11]2[O:12][C:13]([C:16]([N:18]3[CH2:23][CH2:22][N:21]([CH:24]([C:32]4[CH:37]=[CH:36][C:35]([F:38])=[CH:34][CH:33]=4)[C:25]4[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=4)[CH2:20][CH2:19]3)=O)=[CH:14][O:15][C:10]=2[CH:9]=1>C(OCC)C>[OH:7][C:8]1[CH:40]=[CH:39][C:11]2[O:12][C:13]([CH2:16][N:18]3[CH2:19][CH2:20][N:21]([CH:24]([C:32]4[CH:37]=[CH:36][C:35]([F:38])=[CH:34][CH:33]=4)[C:25]4[CH:26]=[CH:27][C:28]([F:31])=[CH:29][CH:30]=4)[CH2:22][CH2:23]3)=[CH:14][O:15][C:10]=2[CH:9]=1

Komponenten

4

Edukt 2

HCID 98044716-Hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylcarbonyl}-1,4-benzodioxinHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 104338936-Hydroxy-2-{4-[bis-(4-fluorophenyl)methyl]piperazin-1-ylmethyl}-1,4-benzodioxinAusbeute 85 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

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%. Melting point: 190° C. ##STR79##

Aufarbeitung

  1. temperatureUnder a nitrogen atmosphere, heat
  2. temperatureAfter cooling
  3. customhydrolysis, removal of the insoluble mineral compounds
  4. filtrationby filtration
  5. dry with materialdrying over magnesium sulfate
  6. customthe compound obtained
  7. customis purified by chromatography on a column of silica (eluant: petroleum ether/ethyl acetate, 40:60)

Quellen und Nachweise

ORD-Eintrag
ord-7ed4eb78a0524eab842045f9adfce8f8
Quelldatensatz
uspto-grants-1995_08
Patentnummer
US05439909

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