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Ethyl Acetate → HCID 18538641, Verbindung

HRID 1394369
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1394369
[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([C:10]([N:12]([C:32]2[CH:37]=[CH:36][C:35]([Cl:38])=[C:34]([Cl:39])[CH:33]=2)[CH2:13][CH2:14][CH2:15][N:16]2[CH2:21][CH2:20][CH:19]([CH2:22][C:23]3[CH:28]=[CH:27][C:26]([N+:29]([O-])=O)=[CH:25][CH:24]=3)[CH2:18][CH2:17]2)=[O:11])[CH2:6][CH2:5]1)(=[O:3])[CH3:2].O=C1NC(CN2CCNCC2)=CC(=O)N1.[OH-].[Na+].C(OCC)(=O)C>C(O)C>[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([C:10]([N:12]([CH2:13][CH2:14][CH2:15][N:16]2[CH2:17][CH2:18][CH:19]([CH2:22][C:23]3[CH:24]=[CH:25][C:26]([NH2:29])=[CH:27][CH:28]=3)[CH2:20][CH2:21]2)[C:32]2[CH:37]=[CH:36][C:35]([Cl:38])=[C:34]([Cl:39])[CH:33]=2)=[O:11])[CH2:6][CH2:5]1)(=[O:3])[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 18538904HCID 18538904, VerbindungHCID 18539274HCID 18539274, Verbindung

Produkt 1

HCID 18538641HCID 18538641, VerbindungAusbeute 92 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702
Ethanol
Lösungsmittel

Versuchsvorschrift

1-Acetyl-N-(3,4-dichlorophenyl)-N-{3-[4-(4-nitrobenzyl)-1-piperidinyl]propyl}-4-piperidinecarboxamide (Example 302)(70 mg, 0.12 mmol) was dissolved in ethanol (0.4 mL). To the mixture was added stannic chloride 2 hydrate (135 mg, 0.61 mmol), and the mixture was heated for 30 minutes under reflux. The mixture was cooled, and to the mixture were added aqueous solution of 1N-sodium hydroxide (10 mL) and ethyl acetate (10 mL). The resulting white precipitates were filtered off with Celite. The filtrate was subjected to extraction procedure. The organic layer was washed with saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The concentrate was subjected to column chromatography (alumina 10 g, ethyl acetate), and the desired fraction was concentrated under reduced pressure to give the titled compound (63 mg, 0.11 mmol, Yield 92%) as pale yellow oily substance.

Aufarbeitung

  1. temperaturethe mixture was heated for 30 minutes
  2. temperatureunder reflux
  3. temperatureThe mixture was cooled
  4. customThe resulting white precipitates
  5. filtrationwere filtered off with Celite
  6. extractionThe filtrate was subjected to extraction procedure
  7. washThe organic layer was washed with saturated aqueous solution of sodium chloride
  8. dry with materialdried over anhydrous sodium sulfate
  9. concentrationconcentrated under reduced pressure
  10. concentrationthe desired fraction was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-926564debd16418cab0b28260d50d312
Quelldatensatz
uspto-grants-2008_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07348324B2

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