Sulfuric Acid → HCID 68707356, Verbindung
Reaktionsgleichung
[H-].[H-].[H-].[H-].[Li+].[Al+3].OS(O)(=O)=O.[ClH:12].[CH3:13][N:14]1[CH2:19][CH2:18][C:17]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)([C:20]#[N:21])[CH2:16][CH2:15]1>C1COCC1>[ClH:12].[ClH:12].[CH3:13][N:14]1[CH2:19][CH2:18][C:17]([CH2:20][NH2:21])([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH2:16][CH2:15]1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
To a solution of LAH (7.5 mmol) in THF (10 mL) is added dropwise conc. H2SO4 (3.8 mmol) at 0° C. After stirred at 0° C. for 0.5 h, 1-methyl-4-phenylpiperidine-4-carbonitrile hydrochloride (2.5 mmol) is added at 0° C. The reaction mixture is stirred at 60° C. for 6 h. After cooled down to 0° C., the reaction is quenched by the addition of Na2SO4-10H2O. The resulting mixture is filtered through celite, and the filtrate is concentrated in vacuo. The residue is suspended in ether and treated with HCl in 1,4-dioxane. The resulting white solid is collected by filtration to give the title compound, which is directly used for the next reaction without further purification.
Aufarbeitung
- stirringThe reaction mixture is stirred at 60° C. for 6 h
- temperatureAfter cooled down to 0° C.
- customthe reaction is quenched by the addition of Na2SO4-10H2O
- filtrationThe resulting mixture is filtered through celite
- concentrationthe filtrate is concentrated in vacuo
- additiontreated with HCl in 1,4-dioxane
- filtrationThe resulting white solid is collected by filtration
Quellen und Nachweise
- ORD-Eintrag
- ord-7317d27a5b354a7994047732e0940f02
- Quelldatensatz
- uspto-grants-2010_04
- Patentnummer
- US07704996B2
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