Water → 1-Acetyl-4-(3-hydroxyphenyl)piperazine

HRID 614433Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 614433
Br.Br.[N:3]1([C:9]2[CH:10]=[C:11]([OH:15])[CH:12]=[CH:13][CH:14]=2)[CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1.O.C(=O)([O-])O.[Na+].[C:22](OC(=O)C)(=[O:24])[CH3:23]>ClC(Cl)Cl>[C:22]([N:6]1[CH2:5][CH2:4][N:3]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([OH:15])[CH:10]=2)[CH2:8][CH2:7]1)(=[O:24])[CH3:23]

Komponenten

6

Edukt 4

HCID 962WaterHCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 198170793-(1-Piperazinyl)phenol dihydrobromide

Produkt 1

HCID 128548521-Acetyl-4-(3-hydroxyphenyl)piperazineAusbeute 70 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Reaktionsbedingungen

Temperatur
10 °C

Versuchsvorschrift

To a stirred solution of 80 parts of 3-(1-piperazinyl)phenol dihydrobromide in 360 parts of water and 180 parts of trichloromethane are added portionwise 42 parts of sodium hydrogen carbonate at 10° C. Then there are added dropwise, during a 15 minutes-period, 26 parts of acetic acid anhydride while cooling at 10° C. Upon completion, stirring is continued for 3 hours at room temperature. The precipitated product is filtered off, washed with water and crystallized from 2-propanol, yielding 37 parts (70%) of 1-acetyl-4-(3-hydroxyphenyl)piperazine; mp. 186.1° C.

Aufarbeitung

  1. filtrationThe precipitated product is filtered off
  2. washwashed with water
  3. customcrystallized from 2-propanol

Quellen und Nachweise

ORD-Eintrag
ord-8e3cd502f96a4db1bf46b343899c4fa2
Quelldatensatz
uspto-grants-1979_03
Patentnummer
US04144346

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