Piperazine → N-(3-benzhydroxypropyl)piperazine

HRID 565633Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 565633
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[C:7]1([CH:13]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[O:14][CH2:15][CH2:16][CH2:17]Br)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>C(O)C.[Na+].[Cl-]>[C:19]1([CH:13]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)[O:14][CH2:15][CH2:16][CH2:17][N:1]2[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]2)[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1

Komponenten

5

Edukt 2

HCID 4837PiperazineHCID 143063671-(Diphenylmethoxy)-3-bromopropane

Produkt 1

HCID 22110970N-(3-benzhydroxypropyl)piperazineAusbeute 99,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittel2×HCID 5234Sodium ChlorideLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

In 20 mL of ethanol was dissolved 20 g of piperazine with heating. Then, a solution of 3-(diphenylmethoxy)propyl bromide (7.0 g) in ethanol (20 mL) was added dropwise and the mixture was stirred at 70° C. for 1 hour. This reaction mixture was diluted with saturated aqueous NaCl and extracted with chloroform. The extract was washed with saturated aqueous NaCl to remove the starting material piperazine, dried over MgSO4, and concentrated under reduced pressure to provide 7.1 g of the title compound. Yield 99%. This product was not further purified but directly submitted to the next reaction.

Aufarbeitung

  1. temperaturewith heating
  2. extractionextracted with chloroform
  3. washThe extract was washed with saturated aqueous NaCl
  4. customto remove the starting material piperazine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-546818fe66f54360b2ea26b4243be733
Quelldatensatz
uspto-grants-2001_01
Patentnummer
US06172085B2

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