2,2-dimethylhexanedinitrile → HCID 11815890, Verbindung

HRID 1699123Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1699123
CC(C)([O-:4])C.[K+].[CH3:7][C:8]([CH3:16])([CH2:11][CH2:12][CH2:13][C:14]#[N:15])[C:9]#N>C1(C)C=CC=CC=1>[C:14]([CH:13]1[C:7](=[O:4])[C:8]([CH3:16])([CH3:9])[CH2:11][CH2:12]1)#[N:15]

Komponenten

4

Edukt 2

HCID 2642192,2-dimethylhexanedinitrileHCID 23665647Potassium tert-butoxide

Produkt 1

HCID 11815890HCID 11815890, VerbindungAusbeute 55 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

A suspension of potassium t-butoxide (60.2 g, 0.54 mole) in toluene is treated with 2,2-dimethyladiponitrile (120.7 g, 0.87 mole) at 80° C., stirred for 2 hours, cooled to less than 30° C., and quenched with water. The phases are separated, the organic phase is stirred with 3N hydrochloric acid and filtered. The filtrate is concentrated in vacuo to give an oil which is distilled (2 torr, 150° C.) twice to afford the title product as a colorless oil, 65.7 g (98.5% pure, 55% yield), identified by gas chromatography.

Aufarbeitung

  1. temperaturecooled to less than 30° C.
  2. customquenched with water
  3. customThe phases are separated
  4. stirringthe organic phase is stirred with 3N hydrochloric acid
  5. filtrationfiltered
  6. concentrationThe filtrate is concentrated in vacuo
  7. customto give an oil which
  8. distillationis distilled (2 torr, 150° C.) twice

Quellen und Nachweise

ORD-Eintrag
ord-4ef161acf469414ba17ef971bbc10a74
Quelldatensatz
uspto-grants-2002_02
Patentnummer
US06344580B1

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