Acetic Acid → 4-[4-(4-Octyloxyphenyl)piperazin-1-yl]benzoic acid

HRID 1386589Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1386589
[CH2:1]([O:9][C:10]1[CH:15]=[CH:14][C:13]([N:16]2[CH2:21][CH2:20][N:19]([C:22]3[CH:29]=[CH:28]C(C#N)=[CH:24][CH:23]=3)[CH2:18][CH2:17]2)=[CH:12][CH:11]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].O.[C:31]([OH:34])(=[O:33])[CH3:32]>OS(O)(=O)=O>[CH2:1]([O:9][C:10]1[CH:15]=[CH:14][C:13]([N:16]2[CH2:21][CH2:20][N:19]([C:22]3[CH:29]=[CH:28][C:32]([C:31]([OH:34])=[O:33])=[CH:24][CH:23]=3)[CH2:18][CH2:17]2)=[CH:12][CH:11]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8]

Komponenten

5

Edukt 3

HCID 176Acetic AcidHCID 962WaterHCID 211822454-[4-(4-Octyloxyphenyl)piperazin-1-yl]benzonitrile

Produkt 1

HCID 211824374-[4-(4-Octyloxyphenyl)piperazin-1-yl]benzoic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

A solution of 4-[4-(4-Octyloxyphenyl)piperazin-1-yl]benzonitrile (0.5 g) in 20% H2SO4 aqueous solution (30 ml) and acetic acid (20 ml) was refluxed for 9 hours. The reaction mixture was pulverized with water. The precipitate was collected by filtration, and added to a mixture of water, tetrahydrofuran and ethyl acetate, and adjusted to pH 2.5 with 1N NaOH aqueous solution. The organic layer was taken, and dried over magnesium sulfate. The magnesium sulfate was filtered off, and the filtrate was evaporated under reduced pressure to give 4-[4-(4-Octyloxyphenyl)piperazin-1-yl]benzoic acid (388 mg).

Aufarbeitung

  1. filtrationThe precipitate was collected by filtration
  2. additionadded to a mixture of water, tetrahydrofuran and ethyl acetate
  3. dry with materialdried over magnesium sulfate
  4. filtrationThe magnesium sulfate was filtered off
  5. customthe filtrate was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-9fdcf6f81db1442c8545cabde755941a
Quelldatensatz
uspto-grants-2001_07
Patentnummer
US06265536B1

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