Acetonitrile → [4-(2-Methoxy-ethyl)-piperazin-1-yl]-benzoic acid methyl ester

HRID 478636Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 478636
COC(=O)[C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)=[CH:6][CH:5]=1.Br[CH2:18][CH2:19][O:20][CH3:21].[C:22](=[O:25])([O-])[O-:23].[K+].[K+].[C:28](#N)C>>[CH3:28][O:23][C:22](=[O:25])[C:6]1[CH:5]=[CH:4][CH:9]=[CH:8][C:7]=1[N:10]1[CH2:11][CH2:12][N:13]([CH2:18][CH2:19][O:20][CH3:21])[CH2:14][CH2:15]1

Komponenten

5

Edukt 4

HCID 6342AcetonitrileHCID 11430Potassium CarbonateHCID 809722-Bromoethyl methyl etherHCID 15429161Methyl 4-(piperazin-1-yl)benzoate

Produkt 1

HCID 69996255[4-(2-Methoxy-ethyl)-piperazin-1-yl]-benzoic acid methyl ester

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

4-(Piperazin-1-yl)-benzoic acid methyl ester (19 mmol), 2-bromoethylmethylether (21 mmol), and potassium carbonate (22.8 mmol) are suspended in acetonitrile (50 ml) and stirred at 80° C. for 8 hours. After evaporation of the solvent, the residue is dissolved in water and extracted three times with CH2Cl2. The extract is dried over sodium sulfate and evaporated. The residue is suspended in diethylether/pentane and the solid filtered of and dried (vacuum). A powder with mp. 103-105° C. is obtained.

Aufarbeitung

  1. customAfter evaporation of the solvent
  2. dissolutionthe residue is dissolved in water
  3. extractionextracted three times with CH2Cl2
  4. dry with materialThe extract is dried over sodium sulfate
  5. customevaporated
  6. filtrationthe solid filtered of and
  7. customdried (vacuum)
  8. customA powder with mp. 103-105° C. is obtained

Quellen und Nachweise

ORD-Eintrag
ord-1cd1d1cbee6746bc99383690b7f9f84c
Quelldatensatz
uspto-grants-2003_11
Patentnummer
US06642239B2

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