Water → HCID 86733843, Verbindung

HRID 2072004Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2072004
[CH2:1]([CH2:8][NH:9][C:10]([CH3:14])([CH3:13])[C:11]#[N:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O>CCOCC>[CH2:1]([CH2:8][NH:9][C:10]([CH3:14])([CH3:13])[CH2:11][NH2:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 962WaterHCID 214098442-Benzylmethylamino-2-methylpropionitrile

Produkt 1

HCID 86733843HCID 86733843, VerbindungAusbeute 55,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

A solution of 2-benzylmethylamino-2-methylpropionitrile (6.7 g.) in ether (100 ml.) was added dropwise to a stirred solution of sodium dihydro bis[2-methoxyethoxy] aluminate (28.5 g.) in ether (150 ml.), kept at 0° C. The mixture was then gently refluxed for 20 hrs, and then excess reducing agent was decomposed by the dropwise addition of water to the cooled suspension. The mixture was dried (anhyd.Na2SO4), filtered (hyflo) and the excess ether evaporated under reduced pressure. The residual liquid was distilled under water pump vacuum to give 2-benzylmethylamino-2-methyl-propylamine (3.8 g.) b.p. 138°-140° C.

Aufarbeitung

  1. customkept at 0° C
  2. temperatureThe mixture was then gently refluxed for 20 hrs
  3. dry with materialThe mixture was dried (anhyd.Na2SO4)
  4. filtrationfiltered (hyflo)
  5. customthe excess ether evaporated under reduced pressure
  6. distillationThe residual liquid was distilled under water

Quellen und Nachweise

ORD-Eintrag
ord-6d48ec0a115741d484345948ad46325e
Quelldatensatz
uspto-grants-1977_09
Patentnummer
US04049663

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