Water → Ethyldiisopropylethylamine

HRID 374668

Reaktionsgleichung

Reaktionsgleichung von HRID 374668
[CH:1]([N:4]([CH:9]([CH3:11])[CH3:10])[CH:5]([CH3:8])[C:6]#N)([CH3:3])[CH3:2].[CH2:12]([Mg]Br)C.O>C(OCC)C>[CH:1]([N:4]([CH:5]([CH2:6][CH3:12])[CH3:8])[CH:9]([CH3:11])[CH3:10])([CH3:3])[CH3:2]

Komponenten

5

Edukt 3

HCID 962WaterHCID 109972602-(Diisopropylamino)propionitrileHCID 178418443HCID 178418443, Verbindung

Produkt 1

HCID 18997630Ethyldiisopropylethylamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

A solution of 2-(diisopropylamino)propionitrile (25.00 g, 0.162 mol) in diethyl ether (20 ml) was added dropwise to a 1M solution of ethyl magnesium bromide in diethyl ether (32.4 ml, 0.324 mol) and the mixture was refluxed for 30 min. Water (25 ml) was added and white precipitate was filtered off and washed with diethyl ether (2×100 ml). The ether solutions were combined, dried over anhydrous magnesium sulfate and the product was isolated by distillation: 13.80 g, 51%, bp 60°-62° C./20 mm Hg. 1H NMR CDCl3 δ ppm, 0.85 (t, J=6.5 Hz, 3H, CH3) , 0.98 (d, J=6.5 Hz, 6H, CH3) 0.99 (d, J=6.5 Hz, 3H, CH3), 1.05 (d, J=6.5 Hz, 6H, CH3) , 1.17-1.44(m, 2H, CH2), 2.70 (m, 1H, CH), 3.08 (sep, J=6.5 Hz, 2H, CH).

Aufarbeitung

  1. temperaturethe mixture was refluxed for 30 min
  2. filtrationwhite precipitate was filtered off
  3. washwashed with diethyl ether (2×100 ml)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe product was isolated by distillation

Quellen und Nachweise

ORD-Eintrag
ord-c0d7bf166159428fb422e6c482e76f6a
Quelldatensatz
uspto-grants-1996_01
Patentnummer
US05481038

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