Sodium sulfate decahydrate → HCID 68644129, Verbindung

HRID 1159187Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1159187
[NH2:1][CH:2]([CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=1)[C:3]#[N:4].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[Cl:13][C:10]1[CH:9]=[CH:8][C:7]([CH2:6][CH2:5][CH:2]([NH2:1])[CH2:3][NH2:4])=[CH:12][CH:11]=1

Komponenten

5

Edukt 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 686441462-Amino-4-(4-chloro-phenyl)-butyronitril

Produkt 1

HCID 68644129HCID 68644129, VerbindungAusbeute 21 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

A solution of 2-amino-4-(4-chloro-phenyl)-butyronitril (0.425 g, 2.18 mmol) in tetrahydrofurane (4 ml) was added dropwise to a suspension of lithium aluminum hydride (0.331 g, 8.73 mmol) in tetrahydrofurane (4 ml) at 0° C. under argon atmosphere. The reaction mixture was allowed to reflux overnight. After cooling to 0° C. solid sodium sulphate decahydrate was added and stirring was continued for 1 hour. The grey suspension was filtered through Celite and the solvent was evaporated. The residue was purified by chromatography (column: Isolute® Flash-NH2 from Separtis; eluent:ethyl acetate/methanol=90:10) to yield a colorless oil (0.091 g, 21%); MS (ISP): 199.1 ((M+H)+).

Aufarbeitung

  1. temperatureto reflux overnight
  2. additionwas added
  3. filtrationThe grey suspension was filtered through Celite
  4. customthe solvent was evaporated
  5. customThe residue was purified by chromatography (column: Isolute® Flash-NH2 from Separtis; eluent:ethyl acetate/methanol=90:10)

Quellen und Nachweise

ORD-Eintrag
ord-d8b7ca91b70e429ba3d9ef52346beb0f
Quelldatensatz
uspto-grants-2010_10
Patentnummer
US07812047B2

Notizen zur Reaktion

Wird geladen…