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Cyanogen Bromide → HCID 87298019, Verbindung

HRID 877854
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 877854
[CH2:1]([NH:3][C:4]1[C:9]([CH3:10])=[CH:8][CH:7]=[CH:6][C:5]=1[CH3:11])[CH3:2].[N:12]#[C:13]Br>C1(C)C=CC=CC=1>[CH2:1]([N:3]([C:13]#[N:12])[C:4]1[C:9]([CH3:10])=[CH:8][CH:7]=[CH:6][C:5]=1[CH3:11])[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 10476Cyanogen BromideHCID 12539332N-Ethyl-2,6-dimethylaniline

Produkt 1

HCID 87298019HCID 87298019, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

N-ethyl-2,6-dimethylaniline (5.9 g, 39.6 mmol) was added to a stirred solution of cyanogen bromide (2.1 g, 19.8 mmol) in toluene (50 mL). The reaction mixture was allowed to react overnight at room temperature during which a solid formed. A small temperature rise to 30° C. was observed. The suspension was filtered and the residue was washed with toluene (3×25 mL). The combined filtrates were evaporated to dryness by rotatory evaporation and the resulting residue was purified by Kugelrohr distillation (0.2 mbar, 110-125° C.) yielding a brown oil. Yield: 3.09 g (90%). The residue (N-ethyl-2,6-dimethylaniline hydrobromide) of the filtration step was used in the following synthetic step.

Aufarbeitung

  1. customto react overnight at room temperature during which a solid
  2. customformed
  3. customto 30° C.
  4. filtrationThe suspension was filtered
  5. washthe residue was washed with toluene (3×25 mL)
  6. customThe combined filtrates were evaporated to dryness by rotatory evaporation
  7. distillationthe resulting residue was purified by Kugelrohr distillation (0.2 mbar, 110-125° C.)
  8. customyielding a brown oil
  9. filtrationThe residue (N-ethyl-2,6-dimethylaniline hydrobromide) of the filtration step

Quellen und Nachweise

ORD-Eintrag
ord-31b0cc3ef0124165a4394cea155ab67f
Quelldatensatz
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08987393B2

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