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Piperidine → HCID 12471526, Verbindung

HRID 2051481
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2051481
Br[C:2]1[CH:3]=[N+:4]([O-:15])[C:5]2[C:10]([C:11]=1[N+:12]([O-:14])=[O:13])=[CH:9][CH:8]=[CH:7][CH:6]=2.[NH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1>O1CCCC1>[N+:12]([C:11]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N+:4]([O-:15])=[CH:3][C:2]=1[N:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1)([O-:14])=[O:13]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 8082PiperidineHCID 84235Quinoline, 3-bromo-4-nitro-, 1-oxide

Produkt 1

HCID 12471526HCID 12471526, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

3-Bromo-4-nitroquinoline-N-oxide (10 g, 0.037 mol) was dissolved in tetrahydrofuran (100 ml). To the solution, piperidine (7.9 g, 0.093 mol) was added and the mixture was stirred at room temperature until gradual crystallization occurred. Tetrahydrofuran was distilled off from the whole reaction mixture under vacuum and the residue was dissolved in chloroform. The chloroform layer was washed with water and dried with anhydrous sodium sulfate. After distilling off the chloroform under vacuum, the residue was washed with a small amount of ethanol and recovered by filtration under vacuum to obtain 4-nitro-3-piperidinoquinoline-N-oxide in an amount of 6.0 g (yield, 59%).

Aufarbeitung

  1. distillationTetrahydrofuran was distilled off from the whole reaction mixture under vacuum
  2. dissolutionthe residue was dissolved in chloroform
  3. washThe chloroform layer was washed with water
  4. dry with materialdried with anhydrous sodium sulfate
  5. distillationAfter distilling off the chloroform under vacuum
  6. washthe residue was washed with a small amount of ethanol
  7. filtrationrecovered by filtration under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-3b5c1d99455d418b9379f07dabe99adc
Quelldatensatz
uspto-grants-1991_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05019574

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