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Diisopropylethylamine → HCID 22989232, Verbindung

HRID 1169025
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1169025
[C:1]1([CH:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[O:8][CH:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[C:22]1[CH:23]=[CH:24][C:25]2[N:26]([N:28]=[CH:29][N:30]=2)[N:27]=1.C(N(C(C)C)C(C)C)C>C(O)CCC>[C:15]1([CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[O:8][CH:9]2[CH2:14][CH2:13][N:12]([C:22]3[CH:23]=[CH:24][C:25]4[N:26]([N:28]=[CH:29][N:30]=4)[N:27]=3)[CH2:11][CH2:10]2)[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1
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Komponenten

5

Edukt 3

HCID 81531DiisopropylethylamineHCID 30175844-BenzhydryloxypiperidineHCID 112406116-Chloro-(1,2,4)triazolo(1,5-b)pyridazine

Produkt 1

HCID 22989232HCID 22989232, VerbindungAusbeute 54,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 2631-ButanolLösungsmittel

Versuchsvorschrift

4-(Diphenylmethoxy)piperidine (1.12 g) and 6-chloro[1,2,4]triazolo[1,5-b]pyridazine (558 mg) were dissolved in 1-butanol (25 ml), followed by addition of N-ethyldiisopropylamine (700 mg). The mixture was refluxed under heating for 17 hours. After being cooled, the mixture was concentrated under reduced pressure. Ice-water was added to the residue, followed by extraction with ethyl acetate. The extract was washed with an aqueous sodium chloride saturated solution, dried over magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography and eluted with a mixture of hexane and ethyl acetate (1:3). Fractions containing the objective compound were collected and recrystallized from ethanol to yield the title compound (757 mg).

Aufarbeitung

  1. temperatureThe mixture was refluxed
  2. temperatureunder heating for 17 hours
  3. temperatureAfter being cooled
  4. concentrationthe mixture was concentrated under reduced pressure
  5. additionIce-water was added to the residue
  6. extractionfollowed by extraction with ethyl acetate
  7. washThe extract was washed with an aqueous sodium chloride saturated solution
  8. dry with materialdried over magnesium sulfate
  9. concentrationconcentrated under reduced pressure
  10. washeluted with a mixture of hexane and ethyl acetate (1:3)
  11. additionFractions containing the objective compound
  12. customwere collected
  13. customrecrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-92087ce920ee4f36a882bbee89f9d7f6
Quelldatensatz
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06627630B1

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