Water → {1-Butyl-4-[1-(1-ethoxy-ethoxy)-2-phenylethyl]cyclohexyl}dimethylamine

HRID 2063722

Reaktionsgleichung

Reaktionsgleichung von HRID 2063722
[CH2:1]([Mg]Cl)[CH2:2][CH2:3][CH3:4].[CH3:7][N:8]([CH3:31])[C:9]1(C#N)[CH2:14][CH2:13][CH:12]([CH:15]([O:23][CH:24]([O:26][CH2:27][CH3:28])[CH3:25])[CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:11][CH2:10]1.O.[Cl-].[NH4+]>O1CCCC1>[CH2:1]([C:9]1([N:8]([CH3:31])[CH3:7])[CH2:14][CH2:13][CH:12]([CH:15]([O:23][CH:24]([O:26][CH2:27][CH3:28])[CH3:25])[CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:11][CH2:10]1)[CH2:2][CH2:3][CH3:4]

Komponenten

6

Edukt 4

HCID 962WaterHCID 25517Ammonium ChlorideHCID 698102431-Dimethylamino-4-[1-(1-ethoxy-ethoxy)-2-phenylethyl]cyclohexanecarbonitrileHCID 178418265HCID 178418265, Verbindung

Produkt 1

HCID 66887575{1-Butyl-4-[1-(1-ethoxy-ethoxy)-2-phenylethyl]cyclohexyl}dimethylamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

A 2 M solution of n-butylmagnesium chloride in tetrahydrofuran (4.62 ml, 9.25 mmol) was added dropwise to a solution of 1-dimethylamino-4-[1-(1-ethoxy-ethoxy)-2-phenylethyl]cyclohexanecarbonitrile (1.06 g, 3.1 mmol) in tetrahydrofuran (15 ml), while cooling with ice and under an argon atmosphere. The mixture was stirred at room temperature for 48 h and thereafter water and saturated ammonium chloride solution (10 ml of each) were added. The phases were separated and the aqueous phase was extracted with diethyl ether (3×10 ml). The combined organic phases were dried with sodium sulfate and concentrated i. vac.

Aufarbeitung

  1. temperaturewhile cooling with ice and under an argon atmosphere
  2. customThe phases were separated
  3. extractionthe aqueous phase was extracted with diethyl ether (3×10 ml)
  4. dry with materialThe combined organic phases were dried with sodium sulfate
  5. concentrationconcentrated i

Quellen und Nachweise

ORD-Eintrag
ord-af4c1f81c53c41e9a8a57f3e86eddcf2
Quelldatensatz
uspto-grants-2012_10
Patentnummer
US08288406B2

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