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Diisobutylaluminum hydride → N1-Methyl-1-phenylethylenediamine

HRID 1092364
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1092364
[CH3:1][NH:2][C:3]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)(C)[C:4]#[N:5].CC(C[AlH]CC(C)C)C>C1(C)C=CC=CC=1>[CH3:1][NH:2][CH:3]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[CH2:4][NH2:5]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 14487Diisobutylaluminum hydrideHCID 137749972-Methylamino-2-phenyl-propionitrile

Produkt 1

HCID 98060N1-Methyl-1-phenylethylenediamineAusbeute 106,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel2×

Versuchsvorschrift

A solution of 2-methylamino-2-phenyl-propionitrile (7.8 g) in toluene (60 mL) was cooled to −78° C. and DIBAL-H solution (104 mL of a 20% solution in toluene) was added drop wise under nitrogen. The reaction mixture was slowly warmed to room temperature and then left at stirring for 17 h. After completion, the reaction mixture was quenched with 30 mL methanol and then 100 mL water. All solvents were evaporated and crude material was taken into 50 mL of water and acidified to pH=1 with 1N HCl. The mixture was extracted with ethyl acetate and separated, and the aqueous layer was basified to pH=14 with 30% NaOH solution. The free diamine was extracted with dichloromethane, dried over sodium sulfate, filtered and concentrated to obtain the desired known N1-methyl-1-phenylethane-1,2-diamine (CAS 66308-14-3) (7.8 g) which was used in the next step without further purification.

Aufarbeitung

  1. waitleft
  2. customAfter completion, the reaction mixture was quenched with 30 mL methanol
  3. customAll solvents were evaporated
  4. extractionThe mixture was extracted with ethyl acetate
  5. customseparated
  6. extractionThe free diamine was extracted with dichloromethane
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-7e12004bca0c4711ab5a21f202882ffe
Quelldatensatz
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08129423B2

Notizen zur Reaktion

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