Acetic Acid → HCID 21558493, Verbindung

HRID 1578693Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1578693
[CH2:1]([N:8]1[CH2:13][CH2:12][C:11](=O)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(O)(=O)C.[NH2:19][C:20]1[CH:25]=[C:24]([Cl:26])[CH:23]=[CH:22][C:21]=1[N:27]1[CH:31]=[CH:30][CH:29]=[CH:28]1>C(O)C>[ClH:26].[CH2:1]([N:8]1[CH2:13][CH2:12][C:11]2([NH:19][C:20]3[C:21](=[CH:22][CH:23]=[C:24]([Cl:26])[CH:25]=3)[N:27]3[CH:28]=[CH:29][CH:30]=[C:31]23)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 176Acetic AcidHCID 192201-Benzyl-4-piperidoneHCID 106554015-chloro-2-(1H-pyrrol-1-yl)aniline

Produkt 1

HCID 21558493HCID 21558493, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

5.29 g (0.028 mole) of 1-benzyl-4-piperidone and 2 ml. of glacial acetic acid are added to a solution of 5.0 g (0.026 mole) of 1-(2-amino-4-chlorophenyl)pyrrole [Example 13(b)] in 80 ml. of absolute ethanol. The solution is refluxed, leaving a yellow oil. The oil is washed with a potassium hydroxide solution, then water, and placed in a refrigerator overnight. The tan solid which forms is dissolved in ether, and ethereal hydrogen chloride is added. The resulting precipitate is washed with water and dried to give 1'-benzyl-7-chloro-4,5-dihydrospiro[pyrrolo(1,2-a)quinoxaline-4,4'-piperidine]hydrochloride, m.p. 282°-283° C.

Aufarbeitung

  1. temperatureThe solution is refluxed
  2. customleaving a yellow oil
  3. washThe oil is washed with a potassium hydroxide solution
  4. customplaced in a refrigerator overnight
  5. dissolutionThe tan solid which forms is dissolved in ether
  6. additionethereal hydrogen chloride is added
  7. washThe resulting precipitate is washed with water
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-1634684d88724983a4033613af82b950
Quelldatensatz
uspto-grants-1976_02
Patentnummer
US03939159

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