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Water → HCID 15485217, Verbindung

HRID 1586463
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1586463
[CH2:1]([N:5]1[CH2:10][CH2:9][N:8]([CH2:11][CH2:12][NH:13][C:14]([C:16]2[C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[N:18]([CH2:25][CH2:26][CH3:27])[N:17]=2)=O)[CH2:7][CH2:6]1)[CH2:2][CH2:3][CH3:4].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>C1COCC1>[CH2:1]([N:5]1[CH2:6][CH2:7][N:8]([CH2:11][CH2:12][NH:13][CH2:14][C:16]2[C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[N:18]([CH2:25][CH2:26][CH3:27])[N:17]=2)[CH2:9][CH2:10]1)[CH2:2][CH2:3][CH3:4]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 962Water2×HCID 14798Sodium HydroxideHCID 15435289HCID 15435289, VerbindungHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 15485217HCID 15485217, VerbindungAusbeute 40,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028
Tetrahydrofuran
Lösungsmittel
2×

Versuchsvorschrift

To a solution of N-[2-(4-n-butyl-1-piperazinyl)-ethyl]-1-n-propylindazole-3-carboxamide (0.36 g) obtained in Example 3 in THF (5 ml) was added lithium aluminum hydride (0.11 g) at room temperature, and the mixture was heated under reflux for 3 hours. The reaction solution was ice-cooled, and were successively added water (0.1 ml), a 15% aqueous sodium hydroxide (0.1 ml), water (0.3 ml) and THF (10 ml). After the reaction solution was stirred at room temperature for 30 minutes, the insolubles were filtered off with Celite. The filtrate was distilled off under reduced pressure, and the residue was purified by thin-layer chromatography on silica gel (chloroform:methanol:aqueous ammonia=8:2:0.2) to give the title compound (0.14 g) as a pale yellow oily substance. Yield=40%.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 3 hours
  3. temperaturecooled
  4. filtrationthe insolubles were filtered off with Celite
  5. distillationThe filtrate was distilled off under reduced pressure
  6. customthe residue was purified by thin-layer chromatography on silica gel (chloroform:methanol:aqueous ammonia=8:2:0.2)

Quellen und Nachweise

ORD-Eintrag
ord-d21c6a4967224611b0b83f84d66d2db1
Quelldatensatz
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05945434

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