1-(2-Methoxyphenyl)piperazine → HCID 13729383, Verbindung

HRID 1906439Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1906439
[C:1]([C:4]1[O:5][C:6]2[C:12]([O:13][CH2:14][CH:15]([OH:18])[CH2:16]Cl)=[CH:11][CH:10]=[CH:9][C:7]=2[CH:8]=1)(=[O:3])[NH2:2].[CH3:19][O:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1[N:27]1[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1.[OH-].[Na+]>O1CCOCC1.C(O)C>[C:1]([C:4]1[O:5][C:6]2[C:12]([O:13][CH2:14][CH:15]([OH:18])[CH2:16][N:30]3[CH2:29][CH2:28][N:27]([C:22]4[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=4[O:20][CH3:19])[CH2:32][CH2:31]3)=[CH:11][CH:10]=[CH:9][C:7]=2[CH:8]=1)(=[O:3])[NH2:2]

Komponenten

6

Edukt 3

HCID 13461-(2-Methoxyphenyl)piperazineHCID 14798Sodium HydroxideHCID 137294082-Carbamoyl-7-(3-chloro-2-hydroxypropoxy)benzofuran

Produkt 1

HCID 13729383HCID 13729383, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

There were dissolved 1.3 g (0.005 mole) of 2-carbamoyl-7-(3-chloro-2-hydroxypropoxy)benzofuran and 1.1 g (0.0055 mole) of 1-(2-methoxyphenyl)piperazine in a mixture solvent of 10 ml of dioxane and 10 ml of ethanol, and the resulting mixture was refluxed with heating for 7 hours. After completion of the reaction, 2N-NaOH solution was added to give the free base, which was extracted from chloroform. The extract was dried with magnesium sulfate. Then, the resultant residue obtained by distilling away the solvent under reduced pressure was crystallized from chloroform and petroleum ether.

Aufarbeitung

  1. temperaturethe resulting mixture was refluxed
  2. temperaturewith heating for 7 hours
  3. additionwas added
  4. customto give the free base, which
  5. extractionwas extracted from chloroform
  6. dry with materialThe extract was dried with magnesium sulfate

Quellen und Nachweise

ORD-Eintrag
ord-a1beb109159c4def9e90f8dcd0ead6f9
Quelldatensatz
uspto-grants-1987_03
Patentnummer
US04652566

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